CN104804231B - 利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶的方法 - Google Patents

利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶的方法 Download PDF

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CN104804231B
CN104804231B CN201510193681.2A CN201510193681A CN104804231B CN 104804231 B CN104804231 B CN 104804231B CN 201510193681 A CN201510193681 A CN 201510193681A CN 104804231 B CN104804231 B CN 104804231B
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filler
ionic liquid
silane
white carbon
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郭宝春
黄晶
唐征海
张立群
卢咏来
孙敏利
张庆华
张宁
董栋
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Beijing RedAvenue Science & Technology Co., Ltd.
Jiaxing Bei Hua pluronic polymer Co., Ltd
South China University of Technology SCUT
Beijing University of Chemical Technology
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Beijing Redavenue Science & Technology Co Ltd
Jiaxing Bei Hua Pluronic Polymer Co Ltd
South China University of Technology SCUT
Beijing University of Chemical Technology
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Abstract

本发明公开了利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶的方法。该方法为：将生胶、填料、硅烷、离子液体依次加入到开炼机或者密炼机中进行混炼得到混炼胶；将上述混炼胶进行高温返炼；返炼后的混炼胶在室温下加入硫化包和防老剂；将混炼胶进行硫化，获得硫化橡胶。本发明方法以离子液体为填料表面硅烷化的催化剂，有效促进白炭黑等浅色填料在橡胶中的分散和橡胶‑填料界面性能，可以大幅降低硅烷用量，大幅提高胎面橡胶材料的动态性能,降低滚动阻力和动态生热，具有工艺简单，不需要添加额外加工设备和步骤的优点，在高性能轮胎的制备中具有重要前景。

Description

利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶 的方法
技术领域
本发明涉及离子液体改性高性能胎面胶的制备方法，具体涉及利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶的方法。
背景技术
以“节油、高安全性和耐久性”为特征的高性能轮胎已成为轮胎工业的最主要发展方向。在胎面胶中引入白炭黑可以显著提高轮胎的抗湿滑性能和降低滚动阻力，已成为高性能胎面胶必不可少的重要填料。为了进一步提高含白炭黑的胎面胶的性能，在轮胎胎面胶的制造中经常使用硅烷化处理，特别是含硫硅烷的硅烷化处理。通过这一作用，白炭黑与橡胶的界面性能得到显著改善。但是，工业上普遍使用含硫硅烷的含量很高(例如占白炭黑用量的10wt％)。众所周知，硅烷在与填料的硅烷化反应过程非常复杂，不仅包括烷氧基与填料表面羟基(例如硅羟基)之间的缩合反应，还包括烷氧基之间的水解和缩合反应，导致硅烷化效率非常低。过高的硅烷用量，不仅增加制造成本，而且与硅烷相关的副反应影响橡胶的性能，同时界面结构的可控性变差。目前，尚没有降低胎面胶制造中硅烷用量和提高硅烷使用效率的有效方法。因此，探索胎面胶制造中硅烷的有效催化方法，可以大大提高硅烷的使用效率和结构的可控性，提高橡胶复合材料的界面性能和填料的分散，从而有效提高胎面胶的动态性能，这对高性能轮胎的制造具有重要的理论意义和现实意义。
离子液体是指熔点在100℃以下的离子熔盐，已经在绿色溶剂、催化、电化学等诸多领域获得了重要的应用。取决于不同的中心原子和取代基，离子液体的正离子部分实际上是一种鎓盐。由于离子液体极性基团与白炭黑表面羟基的作用(例如氢键作用)，它们可以吸附到白炭黑表面。吸附到白炭黑表面的离子液体的鎓离子通过电荷作用可以有效活化硅羟基，即生成硅氧负离子。硅氧负离子的生成是硅氧烷与硅羟基缩合的必要前提步骤。因此，通过离子液体可以显著催化硅氧烷与填料之间的硅烷化反应。
发明内容
本发明目的在于提供促进硅烷与填料反应的方法及基于此作用制备高性能胎面胶的制造方法。本发明基于离子液体的结构设计的灵活性、对硅烷化反应的独特催化作用，通过原位催化作用，可以制备出具有高动态性能的胎面橡胶材料。
本发明目的通过以下技术方案来实现：
利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶的方法，包括以下步骤：
(1)将生胶、填料、硅烷、离子液体依次加入到开炼机或者密炼机中进行混炼得到混炼胶；
(2)将上述混炼胶进行高温返炼；
(3)返炼后的混炼胶在室温下加入硫化包和防老剂；
(4)将混炼胶进行硫化，获得硫化橡胶。
上述方法中，步骤(1)中，所述混炼胶的含胶率为32wt％～42wt％，所述填料包括炭黑和浅色填料，浅色填料占全部填料的比例是10wt％～100wt％，硅烷用量为浅色填料的2wt％～10wt％，离子液体用量为浅色填料的1wt％～8wt％。
上述方法中，所述生胶为天然胶和(或)溶聚丁苯橡胶与顺丁橡胶组成的胎面橡胶的基础橡胶，其中顺丁橡胶优选高顺式顺丁橡胶，其用量占生胶的25～35wt％。
上述方法中，所述填料包括炭黑和浅色填料；所述的浅色填料包括白炭黑、粘土、金属氧化物中的一种或者一种以上的混合物；浅色填料优选白炭黑，白炭黑优选高分散白炭黑；所述的硅烷为含官能团的三烷氧基硅烷，优选通式为含硫硅烷。
上述方法中，所述的离子液体为熔点低于100℃的离子熔盐，包括二烷基咪唑、烷基吡啶或有机磷盐，优选有机磷盐离子液体。
上述方法中，步骤(1)中，所述的混炼的时间为5～10分钟。
上述方法中，步骤(2)中，所述的高温返炼在开炼机或者密炼机中进行，温度为125～155℃，时间5～15分钟。
上述方法中，所述的硫化包是指以硫磺配合硫化活化剂和促进剂、或过氧化物配合活化剂、或硫磺复配过氧化物体系。
上述方法中，所述的防老剂包括对苯二胺类和喹啉类中的一种以上。
步骤(3)中所述的硫化包是以硫磺为主要硫化剂，以次磺酰胺为主要促进剂的硫化体系，硫化剂的具体种类和用量更加生成需要确定。防老剂是指胎面橡胶常见的防老剂，优选对苯二胺类和(或)喹啉类防老剂。
本发明的基本原理如下：离子液体的正离子可以通过电荷作用活化浅色填料的表面羟基，例如硅羟基。因此，在离子液体作用下，硅氧负离子的浓度有效增加，烷氧基与硅羟基之间的缩合效率大大增加。通过有效提高的界面化学反应，白炭黑的分散程度和界面相互作用提高，硫化橡胶的静态性能(特别是模量)和动态性能显著改善。因此，通过这一方法可以制备高性能的胎面橡胶材料。
与传统工艺技术相比，本发明具有如下优点：
(1)本发明在原有橡胶加工过程中原位实施，不会增加额外的加工设备或者步骤。
(2)离子液体具有丰富的结构多样性，因此，本发明所述的催化效果和橡胶动态性能的调节可以通过改变离子液体的结构方便地进行调节。
(3)本发明所述方法可以降低硅烷用量，降低成本，大幅提升胎面橡胶的动态性能，在高性能轮胎的制造中具有非常广泛的应用前景。
具体实施方式
下面结合具体实施例对本发明作进一步地具体详细描述，但本发明的实施方式不限于此，对于未特别注明的工艺参数，可参照常规技术进行。
(1)将生胶、填料、硅烷、离子液体依次加入到开炼机进行混炼，时间为10分钟得到混炼胶；
(2)将上述混炼胶进行高温返炼；
(3)返炼后的混炼胶在室温下加入必要的硫化体系和防老体系；
(4)将混炼胶进行硫化，获得硫化橡胶。
步骤(2)中所述的高温返炼在开炼机中进行，混炼温度为145℃，混炼时间8分钟。
步骤(4)所述的硫化是指在150℃下按表2中的正硫化时间进行硫化。
为了验证本发明所述方法的优点，选取一个以溶聚丁苯和顺丁橡胶为基础橡胶的轮胎胎面橡胶配方，选用不同的硅烷和离子液体种类及含量，按照本发明上述方法制备了对比样和4个实施例。具体配方如表1,表中单位均为g。
表1对比样和实施例配方表
按照相应的中国国家标准全面测试了所有配方的性能，其典型性能列于表2中。表2显示，本发明所述方法可以显著降低胎面胶的滚动阻力(以60℃下的tan delta表示)和动态生热，可以显著提高硫化橡胶的模量。同时，配方中硅烷的用量大大降低。
表2对比样和实施例所述样品的典型性能
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。

Claims (10)

1.利用离子液体原位催化填料的硅烷化反应制备高性能胎面胶的方法，其特征在于，包括以下步骤：
（1）将生胶、填料、硅烷、离子液体依次加入到开炼机或者密炼机中进行混炼得到混炼胶；
（2）将上述混炼胶进行高温返炼；
（3）返炼后的混炼胶在室温下加入硫化包和防老剂；
（4）将混炼胶进行硫化，获得硫化橡胶；
所述填料包括炭黑和浅色填料，浅色填料包括白炭黑、粘土或金属氧化物中的一种以上，所述的硅烷为含官能团的三烷氧基硅烷，所述含官能团的三烷氧基硅烷的通式为含硫硅烷。
2.根据权利要求1所述的方法，其特征在于，步骤（1）中，所述混炼胶的含胶率为32 wt%~42 wt%，所述浅色填料占全部填料的比例是10 wt%~100 wt%，硅烷用量为浅色填料的2wt%~10 wt %，离子液体用量为浅色填料的1 wt%~8 wt %；所述浅色填料占全部填料的比例不为100 wt%。
3.根据权利要求1所述的方法，其特征在于，所述生胶为天然胶和溶聚丁苯橡胶与顺丁橡胶组成的胎面橡胶的基础橡胶，其中顺丁橡胶为高顺式顺丁橡胶，其用量占生胶的25~35wt%。
4.根据权利要求1所述的方法，其特征在于，所述生胶为天然胶或溶聚丁苯橡胶与顺丁橡胶组成的胎面橡胶的基础橡胶，顺丁橡胶用量占生胶的25~35 wt%。
5.根据权利要求1所述的方法，其特征在于，所述白炭黑为高分散白炭黑。
6.根据权利要求1所述的方法，其特征在于，所述的离子液体为熔点低于100℃的离子熔盐，包括二烷基咪唑、烷基吡啶或有机磷盐。
7.根据权利要求1所述的方法，其特征在于，步骤（1）中，所述混炼的时间为5~10分钟。
8.根据权利要求1所述的方法，其特征在于，步骤（2）中，所述的高温返炼在开炼机或者密炼机中进行，温度为125~155℃，时间5~15分钟。
9.根据权利要求1所述的方法，其特征在于，所述的硫化包是指以硫磺配合硫化活化剂和促进剂、或过氧化物配合活化剂、或硫磺复配过氧化物体系。
10.根据权利要求1所述的方法，其特征在于，所述的防老剂包括对苯二胺类和喹啉类中的一种以上。
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