Huang Zhiyong, Zhu Huixin, Jin Guofeng, Huang Yuanzheng, Gao Minna
Xi'an Institute of High Technology Xi'an 710000 China
RSC Adv. 2022 Jun 21;12(28):18215-18223. doi: 10.1039/d2ra02693g. eCollection 2022 Jun 14.
A thiourea modified low molecular weight polyamide (TLMPA) as a room temperature curing agent was synthesized by a two-step method. Firstly, a low molecular weight polyamide curing agent (LMPA) with low viscosity and high amine value was synthesized by amidation of sebacic acid with tetraethylenepentamine, then the synthesized curing agent was modified with thiourea to increase its reactivity at room temperature. The optimal reaction conditions were studied by L(3) orthogonal experiments. The structure of the prepared curing agent was analyzed by Fourier transform infrared spectroscopy (FT-IR). The kinetics of TLMPA curing of E-51 epoxy resin was analyzed using the Kissinger method with non-isothermal differential scanning calorimetry (DSC). The activation energy of TLMPA/E-51 calculated by the Kissinger method and FWO method was 38.79 kJ mol and 42.73 kJ mol. The nano-SiO filler was compounded with E-51 epoxy resin, TLMPA, allyl glycidyl ether diluent, and KH-560 coupling agent to prepare the room temperature curing epoxy resin (EP) system. L(3) orthogonal experiments were carried out to study the effect of various factors on the mechanical properties of the cured resin systems. The best formulation of the system is that the content of nano-SiO, curing agent, diluent, and coupling agent is 3, 35, 15, 1 wt%, respectively. With the optimal formulation, the tensile and shear strength, tensile strength, impact strength, and bending strength of the cured EP system was 13.19 MPa, 53.8 MPa, 52.16 kJ m, and 94.95 MPa, respectively.
采用两步法合成了一种作为室温固化剂的硫脲改性低分子量聚酰胺(TLMPA)。首先,通过癸二酸与四乙烯五胺的酰胺化反应合成了低粘度、高胺值的低分子量聚酰胺固化剂(LMPA),然后用硫脲对合成的固化剂进行改性,以提高其室温反应活性。通过L(3)正交实验研究了最佳反应条件。采用傅里叶变换红外光谱(FT-IR)对制备的固化剂结构进行了分析。使用非等温差示扫描量热法(DSC)的基辛格方法分析了TLMPA固化E-51环氧树脂的动力学。通过基辛格方法和FWO方法计算得到的TLMPA/E-51的活化能分别为38.79 kJ/mol和42.73 kJ/mol。将纳米SiO填料与E-51环氧树脂、TLMPA、烯丙基缩水甘油醚稀释剂和KH-560偶联剂进行复合,制备了室温固化环氧树脂(EP)体系。通过L(3)正交实验研究了各种因素对固化树脂体系力学性能的影响。该体系的最佳配方为纳米SiO、固化剂、稀释剂和偶联剂的含量分别为3、35、15、1 wt%。采用最佳配方时,固化EP体系的拉伸强度、剪切强度、拉伸模量、冲击强度和弯曲强度分别为13.19 MPa、53.8 MPa、52.16 kJ/m²和94.95 MPa。