CN115028966A - 宽温度域热塑性超韧弹性体树脂组合物 - Google Patents
宽温度域热塑性超韧弹性体树脂组合物 Download PDFInfo
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- CN115028966A CN115028966A CN202210841881.4A CN202210841881A CN115028966A CN 115028966 A CN115028966 A CN 115028966A CN 202210841881 A CN202210841881 A CN 202210841881A CN 115028966 A CN115028966 A CN 115028966A
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Abstract
本发明通常涉及弹性体树脂组合物；更优选涉及一种宽温度域热塑性超韧聚氨酯‑环氧树脂组合物，解决了现有技术中聚氨酯弹性体耐水性、耐水解、耐湿热老化以及耐候性差和环氧树脂柔韧性、耐候性以及耐疲劳性能差等问题。在一个具体实施方式中，由聚醚(酯)多元醇、多异氰酸酯和二醇(胺)扩链剂经反应制备的聚氨酯类超韧弹性体和由环氧树脂和环氧固化剂反应制备的环氧类超韧树脂组合物。在多个具体实施方式中，本发明超韧弹性体组合物在100～200℃之间具有很好的熔融特性，该宽温度域热塑性超韧弹性体树脂组合物主要用于道路交通技术产业领域，具有优异的高温稳定性、耐水性、常温抗疲劳以及低温抗开裂性能。
Description
技术领域
本发明涉及一种热塑性弹性体树脂组合物；更优选涉及宽温度域热塑性超韧弹性体树脂组合物。在多个具体实施方式中，本发明的超韧弹性体组合物在100～200℃之间具有很好的熔融特性，同时仍然保持着良好的综合热力学性能。在一个具体实施方式中，由双酚A型环氧树脂、增韧剂和环氧固化剂的反应制备本发明的环氧类超韧树脂组合物。在一个具体实施方式中，由聚醚(酯)多元醇、多异氰酸酯和二醇(胺)扩链接的反应制备本发明的聚氨酯类超韧弹性体树脂组合物。在另一个具体实施方式中，由聚醚(酯)多元醇、多异氰酸酯和二醇(胺)扩链接的反应制备聚氨酯类超韧弹性体和由双酚A型环氧树脂、增韧剂和环氧固化剂的反应制备本发明的环氧类超韧树脂组合物。
背景技术
聚氨酯结构中由于兼具硬链段部分和软链端部分而使其不但具有极其突出的强度与韧性、良好的耐温性、耐蠕变性、耐磨性、及抗冲击性，而且具有优异的耐低温型、耐化学品性、抗老化性；被广泛应用于交通运输、建筑、机械、电子设备、家具、食品加工、纺织服装、合成皮革、印刷、矿冶、石油化工、水利、国防、体育、医疗等领域。然而，缺点依然很明显，聚氨酯弹性体材料中使用的原材料，比如聚醚多元醇、聚酯多元醇以及多异氰酸酯均对水汽敏感，成型的聚氨酯弹性体耐水解、耐水性、耐湿热老化性能均较差。
环氧树脂是一个分子中含有两个以上环氧基，并在适当的化学试剂存在下能形成三维交联网络状固化物的化合物总称。环氧树脂通常是在呈液体状态下使用的，经常温或加热进行固化，达到最终的使用目的，具有收缩率小，粘结强度高、耐腐蚀、耐化学药品性以及力学性能和电气性能优良的特点，被广泛应用于多种金属与非金属的粘结、耐腐蚀涂料、电气绝缘材料、玻璃钢/复合材料等制造。其缺点是耐候性、韧性以及耐疲劳性能差。
因此，制备获得具有优异的力学性能，大幅降低聚氨酯弹性体耐水性、耐水解、耐湿热老化、耐候性，提高环氧树脂韧性以及耐疲劳性能差等问题，并拥有宽温度域内热塑性树脂特性的组合物，该热塑性超韧弹性体树脂颗粒的应用，主要用于道路交通产业领域。
发明内容
本申请实施例通过提供一种宽温度域热塑性超韧弹性体树脂组合物，解决了现有技术中聚氨酯弹性体耐水性、耐水解、耐湿热老化以及耐候性差和环氧树脂柔韧性、耐候性以及耐疲劳性能差等问题；该热塑性超韧弹性体树脂组合物具有较低熔点，在100～200℃内可以与道路交通材料，比如沥青，很好的熔融混合均匀，即使掺量高达50％时，依然具有良好的施工操作性能。然而，和本发明热塑性超韧性弹性体树脂相比，其他的热塑性材料，比如SBS，PE，EVA，SEBS等掺量大于10％时，黏度急剧增加，完全丧失了流动性，只有大幅提高温度才可能具备一定的施工操作性能。本发明适用于浇注式沥青改性剂、热拌沥青改性剂、温拌沥青改性剂，掺量高达10～50％，力学性能极佳，具有优异的高温稳定性、常温抗疲劳、低温抗开裂性能。
为解决上述技术问题，本发明采用如下技术方案：
本发明的宽温度域热塑性超韧弹性体树脂组合物，可选择一种或几种环氧类超韧树脂、一种或几种聚氨酯类超韧弹性体、或者它们中任意一种或几种适当的组合物。
进一步的，环氧类超韧树脂，包括以下物质的反应产物：
(a)至少一种双酚A型环氧树脂，其优选自一种或几种环氧值为0.12，0.2，0.3，0.42，0.44，0.51，0.54的双酚A型环氧树脂；进一步，具体的，比如E-12，E-20，E-30，E-42，E-44，E-51，E-54；和
(b)至少一种环氧树脂固化剂，其优选自胺类(比如，聚醚胺M2070，M-2005，M600等；比如脂肪胺，十二胺，十四胺，十六胺等)、醇类(比如，乙二醇，1,4-丁二醇，聚乙二醇，聚丙二醇等)、酚类(比如，二酚基丙烷，氢化双酚A)、酸类(比如，己二酸，癸二酸，二聚酸等)、异氰酸酯类(比如，2,6-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯等)中任意一种。
在以下多个具体的实施方式中，环氧树脂官能团环氧基与环氧固化剂官能团摩尔比为0.90～1.1，或甚至为0.95～1.05。
进一步的，聚氨酯类超韧弹性体，包括以下物质的反应产物：
(a)至少一种聚酯多元醇，其优选自一种或几种聚己二酸酯二醇、一种或几种聚碳酸酯二醇、一种或几种聚己内酯二醇、或它们中任意一种或几种的组合物，且其数均分子量为200～1000；
(b)至少一种多异氰酸酯，其优选自2,6-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、1,6-亚己基二异氰酸酯中任意一种或几种的组合物，且其单体有效含量不小于97.5％；和
(c)至少一种伯胺扩链剂，其优选自一种或几种脂肪伯胺、一种或几种聚醚伯胺，或它们中任意一种或几种的组合物，且其中脂肪胺扩链剂，其数均分子量约为100～300，聚醚伯胺，其数均分子量为200～2000；
进一步的，聚氨酯类超韧弹性体，包括以下物质的反应产物：
(a)至少一种聚醚多元醇，其优选自一种或几种聚氧化丙烯二醇、一种或几种聚四氢呋喃二醇、一种或几种双酚A聚氧化乙烯醚、或它们中任意一种或几种的组合物，且其数均分子量约为1000～3000；
(b)至少一种多异氰酸酯，其优选自2,6-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、1,6-亚己基二异氰酸酯、四甲基间苯二亚甲基二异氰酸酯、二甲基联苯二异氰酸酯、二环己基甲烷二异氰酸酯中任意一种，且其单体有效含量不小于97.5％；和
(c)至少一种二醇扩链剂，其优选自1,4-丁二醇、乙二醇、1,6-己二醇、对苯二酚二羟乙基醚、双酚A、对双羟乙基双酚A中任意一种或几种的组合物；
除了上述确定组分外，本发明超韧聚氨酯弹性体树脂组合物还可以任选多种添加剂、颜料、紫外线吸收剂、抗氧化老化剂、催化剂等，掺量参照本领域或文献中已知的常规用量。在以下多个具体的实施方式中，多异氰酸酯官能团与混合聚醚/聚酯多元醇以及扩链剂的全部基团摩尔比为0.95～1.05，或为0.99～1.01，或甚至为1.0。
一种宽温度域热塑性环氧类超韧树脂，由至少一种环氧树脂和至少一种环氧固化剂的反应物形成。
一种宽温度域热塑性聚氨酯类超韧弹性体，由至少一种聚酯多元醇、至少一种多异氰酸酯和至少一种伯胺扩链剂的反应物形成。
一种宽温度域热塑性聚氨酯类超韧弹性体，由至少一种聚醚多元醇、至少一种多异氰酸酯和至少一种二醇扩链剂的反应物形成。
一种宽温度域热塑性超韧弹性体树脂，由至少一种环氧树脂和至少一种环氧固化剂的反应物和至少一种聚酯多元醇、至少一种多异氰酸酯和至少一种伯胺扩链剂的反应物形成。
一种宽温度域热塑性超韧弹性体树脂，由至少一种环氧树脂和至少一种环氧固化剂的反应物和至少一种聚醚多元醇、至少一种多异氰酸酯和至少一种二醇扩链剂的反应物形成。
本发明的宽温度域热塑性聚氨酯超韧弹性体树脂可以为任何所需的最终产物或形式，或直接冷却至室温、或造粒、或造粒用于储存或以大块状运输。或者挤出后立即以其他方式处理挤出物，以获得最终所需的产品。
一种宽温度域热塑性超韧弹性体树脂组合物，其使用温度范围为100～200℃；该温度域内热塑性超韧弹性体树脂主要用于道路交通产业领域，通常用作沥青改性剂使用，即按照一定掺量加入至沥青中，搅拌混合均匀即可。
本申请实施例中提供的一个或多个技术方案，至少具有如下技术效果或优点：
1.由于采用了二步反应高温熔融嵌段接枝技术手段，一步反应获得具有端反应活性基团的环氧超韧树脂反应物，比如端环氧基、端氨基、端羟基、端羧基；聚氨酯弹性体中含有的端活性反应基团为端异氰酸酯基，端羟基；二步反应为环氧超韧树脂反应物中的反应性端基与聚氨酯弹性体反应物中的反应性端基之间接枝反应，最终获得性能优异的热塑性嵌段式超韧聚氨酯弹性体-环氧树脂反应产物，有效解决了现有技术中聚氨酯耐水性、耐水解性、耐湿热老化性能差以及环氧树脂韧性、抗疲劳性能以及耐候性差的技术问题，进而大幅改善了聚氨酯弹性体的耐水性，耐水解性同时聚氨酯弹性体弥补了环氧树脂韧性不足的最大缺陷，获得了柔韧性优异且耐水性和耐水解性能良好的热塑性超韧聚氨酯弹性体树脂组合物。
2.本发明热塑性超韧聚氨酯弹性体树脂组合物，平时分开反应获得任何形式的产品，比如块状、颗粒、粉末等，使用时按照环氧超韧树脂与聚氨酯超韧弹性体按照一定的比例添加至沥青中，施工温度下熔融搅拌均匀即可，沥青相当于溶剂，使得熔融态环氧树脂反应物和聚氨酯弹性体反应物进行进一步的接枝反应的发生，使用方便，施工方法简单。
3.本发明热塑性超韧聚氨酯弹性体树脂组合物，熔融温度低；用作道路交通沥青改性剂，在100～200℃时掺量高达10％～50％，是一般SBS、SEBS、EVA等改性剂掺量的2～10倍，大幅提升沥青的综合热力学性能，尤其是不影响施工可操作性能。
4.本发明热塑性超韧聚氨酯弹性体树脂组合物，掺量为大于35％时，沥青作为分散相填充于连续相聚氨酯弹性体树脂网络中，拉伸性能大于2MPa，延伸率大于200％，拉伸过程无颈缩现象，属于性能优异的弹性体，满足性能要求苛刻的钢桥面铺装材料要求。
5.本发明热塑性超韧聚氨酯弹性体树脂组合物，掺量为10％～35％时，聚氨酯弹性体树脂作为分散相填充于沥青连续相中，拉伸性能小于0.5～2MPa，延伸率大于200％，拉伸过程出现颈缩现象，但是可以满足除钢桥面铺装材料外的其他铺装材料要求，比如高速公路、机场跑道、城市立交桥、市政道路等道路等级要求高的场合。
6.本发明热塑性超韧聚氨酯弹性体树脂组合物，环氧树脂与聚氨酯弹性体比值越大，力学性能越好，韧性逐渐变差；反之，其比值越小，力学性能逐渐变差，但韧性越来越好。
附图说明
图1为本申请实施例22中掺量为20％，30％，35％，45％时改性沥青微观图像。
具体实施方式
本发明不受下述实施例的限制，可根据本发明的技术方案与实际情况来确定具体的实施方式。本发明中所提到的化学试剂或化学品如无特殊说明，均为现有技术中公用的化学试剂、或化学品、或工业品。其他未注明的试验方法或试验设备均为本行业技术人员已知通用的试验方法和试验设备。
为了更好的理解上述技术方案，下面将结合说明书以及具体的实施方式对上述技术方案进行详细的说明。表1和表2分别举例说明了多种环氧树脂配方和多种聚氨酯弹性体配方，即对比实施例1～7和对比实施例8～14。表3为该宽温度域热塑性超韧弹性体树脂单独实际应用效果，即对比例15～21。表4为该宽温度域热塑性超韧弹性体树脂组合物之间配合使用时的应用效果。
以下获得的环氧类超韧树脂和聚氨酯类超韧弹性体均是通过无规熔融聚合方法制备的。该方法中，对于环氧类超韧树脂，在50～80℃下将环氧树脂组分和环氧固化剂组分混合在一起，然后逐渐升温至110～180℃，持续反应0.5～3小时，期间保持持续的搅拌，即得到本发明所述的环氧类超韧树脂。对于聚氨酯类超韧弹性体，在100～130℃下混合，在装有搅拌器的反应釜中持续搅拌1～3min，即得到聚氨酯类超韧弹性体。
表1
表2
表3
1：指的是单独使用表1和表2对应实施例获得的热塑性超韧弹性体树脂作为改性剂试验结果
表4
2：指的是使用表1和表2对应实施例获得热塑性超韧弹性体树脂组合物试验结果
尽管已描述了本发明的优选实施例，但本领域内的技术人员一旦得知了基本创造性概念，则可对这些实施例作出另外的变更和修改。所以，所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。
Claims (10)
1.宽温度域热塑性超韧弹性体树脂组合物，其特征在于：可选择一种或几种环氧类超韧树脂、一种或几种聚氨酯类超韧弹性体、或者它们中任意一种或几种适当的组合物。
2.如权利要求1所述宽温度域热塑性超韧弹性体树脂组合物，其特征在于，所述环氧类超韧树脂，包括以下物质的反应产物：
(a)至少一种双酚A型环氧树脂，其优选自一种或几种环氧值为0.12，0.2，0.3，0.42，0.44，0.51，0.54的双酚A型环氧树脂；和
(b)至少一种环氧树脂固化剂，其优选自胺类、醇类、酚类、酸类、异氰酸酯类中任意一种。
3.如权利要求1、2所述宽温度域热塑性超韧弹性体树脂组合物，其特征在于，所述聚氨酯类超韧弹性体，包括以下物质的反应产物：
(a)至少一种聚酯多元醇，其优选自一种或几种聚己二酸酯二醇、一种或几种聚碳酸酯二醇、一种或几种聚己内酯二醇、或它们中任意一种或几种的组合物；
(b)至少一种多异氰酸酯，其优选自2,6-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、1,6-亚己基二异氰酸酯中任意一种或几种的组合物；和
(c)至少一种伯胺扩链剂，其优选自一种或几种脂肪伯胺、一种或几种聚醚伯胺，或它们中任意一种或几种的组合物；
其中至少一种聚酯多元醇，其数均分子量为200～1000；其中至少一种多异氰酸酯，其单体有效含量不小于97.5％；和其中至少一种脂肪胺扩链剂，其数均分子量约为100～300，一种或几种聚醚伯胺，其数均分子量为200～2000。
4.如权利要求1、2、3所述宽温度域热塑性超韧弹性体树脂组合物，其特征在于，所述聚氨酯类超韧弹性体，包括以下物质的反应产物：
(a)至少一种聚醚多元醇，其优选自一种或几种聚氧化丙烯二醇、一种或几种聚四氢呋喃二醇、一种或几种双酚A聚氧化乙烯醚、或它们中任意一种或几种的组合物；
(b)至少一种多异氰酸酯，其优选自2,6-甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、1,6-亚己基二异氰酸酯、四甲基间苯二亚甲基二异氰酸酯、二甲基联苯二异氰酸酯、二环己基甲烷二异氰酸酯中任意一种；和
(c)至少一种二醇扩链剂，其优选自1,4-丁二醇、乙二醇、1,6-己二醇、对苯二酚二羟乙基醚、双酚A、对双羟乙基双酚A中任意一种或几种的组合物；
其中至少一种聚醚多元醇，其数均分子量约为1000～3000；其中至少一种多异氰酸酯，其单体有效含量不小于97.5％。
5.一种宽温度域热塑性环氧类超韧树脂，由权利要求2所述的组合物形成。
6.一种宽温度域热塑性聚氨酯类超韧弹性体，由权利要求3所述的组合物形成。
7.一种宽温度域热塑性聚氨酯类超韧弹性体，由权利要求4所述的组合物形成。
8.一种宽温度域热塑性超韧弹性体树脂，由权利要求2所述的组合物和由权利要求3所述的组合物形成。
9.一种宽温度域热塑性超韧弹性体树脂，由权利要求2所述的组合物和由权利要求4所述的组合物形成。
10.如权利要求1～9中任一项所述的宽温度域热塑性超韧弹性体树脂组合物，其使用温度范围为100～200℃；该热塑性超韧弹性体树脂主要用于道路交通产业领域。
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