硅烷偶联剂改性白炭黑及在硅橡胶中的应用

发布时间：2019-01-26 15:11

【摘要】：本论文主要研究了两大类硅烷偶联剂改性纳米白炭黑(SiO2)改性过程,并将改性后的白炭黑填充到硅橡胶中,考察对比了不同结构硅烷偶联剂改性后的白炭黑对硅橡胶力学性能的影响。论文首先合成了三类新型α-官能团硅烷偶联剂:以氯甲基三氯硅烷为基本原料,通过醇解制备得到氯甲基三甲氧基硅烷,首先通过甲基丙烯酸钾盐和氯甲基三甲氧基硅烷间的亲核取代反应,合成了甲基丙烯酰氧甲基三甲氧基硅烷(α-570);其次以乙二胺和氯甲基三甲氧基硅烷为原料,在一定条件下,通过胺解反应制备得到N-(β-氨乙基)-氨甲基三甲氧基硅烷(α-DAMO);最后,通过硫脲与氯甲基三甲氧基硅烷进行反应制取得到了巯甲基三甲氧基硅烷(α-590)。通过对上述产物进行红外光谱(FT-IR)和核磁共振氢谱(1H-NMR)表征和分析,证实了得到的产物确实为预期α-官能团硅烷结构。然后作者利用两种不同的改性手段对传统型硅烷偶联剂与上述合成的新硅烷偶联剂对纳米白炭黑表面进行实验。发现不预先水解直接添加到溶剂体系中反应的改性效果更加优异。其主要实验方法是:在以无水甲苯为溶剂体系的纳米白炭黑混合液中,直接添加一定量的硅烷偶联剂,在一定条件下反应,得到硅烷偶联剂改性的纳米白炭黑。通过这种试验方法,分别采用不同种类的硅烷偶联剂(γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(KH-560)、γ-(甲基丙烯酰氧基)丙基三甲氧基硅烷(KH-570)、γ-(N-β-氨乙基)-氨甲基三甲氧基硅烷(DAMO)、α-570和α-DAMO)改性纳米白炭黑,并将得到的改性产物进行FT-IR表征。最后作者对硅烷偶联剂改性纳米白炭黑对硅橡胶性能影响研究。将不同种类和质量改性的纳米白炭黑,作为填料添加到硅橡胶中,改变配方,进行混炼、硫化,得到高温硫化的硅橡胶胶片,将得到的胶片进行力学性能检测,分析改性炭黑填充的硅橡胶在硬度、拉伸强度、拉断伸长率和撕裂强度等方面的影响,将硅橡胶胶样进行扫描电子显微镜(SEM)表征,观察并对比不同改性的纳米白炭黑粒子在硅橡胶中的分散程度。
[Abstract]:In this paper, the modification process of nano-silica (SiO2) modified by two kinds of silane coupling agents was studied, and the modified silica was filled into silicone rubber. The effect of silica modified with silane coupling agent on the mechanical properties of silicone rubber was investigated. In this paper, three kinds of new 伪 -functional silane coupling agents were synthesized firstly. Chloromethyl trichlorosilane was synthesized by alcoholysis to prepare chloromethyl trimethoxy silane from chloromethyl trichlorosilane. Firstly, methacryloxymethyl trimethoxysilane (伪 -570) was synthesized by nucleophilic substitution reaction between potassium methacrylate and chloromethyltrimethoxysilane. Secondly, using ethylenediamine and chloromethyltrimethoxysilane as raw materials, N- (尾 -aminoethyl) -aminomethyltrimethoxysilane (伪-DAMO);) was prepared by amination reaction under certain conditions. Finally, mercapto trimethoxysilane (伪 -590) was prepared by reaction of thiourea with chloromethyl trimethoxysilane. The products were characterized and analyzed by infrared spectroscopy (FT-IR) and nuclear magnetic resonance (1H-NMR). Then two different modification methods were used to study the effect of traditional silane coupling agent and the new silane coupling agent on the surface of nanometer silica. It was found that the modification effect of adding directly to the solvent system without pre-hydrolysis was more excellent. The main experimental methods are as follows: Nano-silica modified by silane coupling agent can be obtained by adding a certain amount of silane coupling agent directly in the mixture of nano-silica with anhydrous toluene as solvent. Different silane coupling agents (纬-(2o 3- epoxypropoxy) propyl trimethoxy silane (KH-560), 纬-(methacryloxy) propyl trimethoxysilane (KH-570), respectively) were used. 纬-(N- 尾 -aminoethyl) -aminomethyltrimethoxysilane (DAMO), 伪 -570 and 伪-DAMO) were used to modify nano-silica, and the modified products were characterized by FT-IR. Finally, the effect of silane coupling agent modified nano silica on the properties of silicone rubber was studied. Nano-silica modified by different kinds and quality was added to silicone rubber as filler, the formula was changed, mixed, vulcanized, high temperature vulcanized silicone rubber film was obtained, and the mechanical properties of the obtained film were tested. The effects of modified carbon black filled silicone rubber on hardness, tensile strength, tensile elongation and tear strength were analyzed. The silicone rubber samples were characterized by scanning electron microscopy (SEM). The dispersion degree of different modified silica nanoparticles in silicone rubber was observed and compared.
【学位授予单位】：济南大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ127.2;TQ333.93

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