Li Ping, Wang Xiaochuan
School of Mechanical and Electronic Engineering, Guangzhou University, Guangzhou 510006, China.
School of Biomedical Sciences and Engineering, Guangzhou International Campus, South China University of Technology, Guangzhou 511442, China.
Materials (Basel). 2022 May 9;15(9):3396. doi: 10.3390/ma15093396.
As a significant component of composite solid propellants, the cross-link alkenyl polymers need to cure at high temperatures and the current isocyanate curing systems are highly humidity sensitive. This paper presented a low-temperature curing method for a cross-linked polymer (polybutadiene) with stable wettability by using cycloaddition of the nitrile oxide of tetramethyl-terephthalobisnitrile oxide (TTNO) and the C=C group of liquid polybutadiene (PB). The TTNO was synthesized in four steps from 1,2,4,5-tetramethylbenzene and evaluated as a low-temperature hardener for curing liquid PB. To characterize the reaction ability of TTNO at 25 °C, the cross-linked rubber materials of various contents (8%, 10%, 12%, 14%, 16%) of curing agent TTNO were prepared. The feasibility of the curing method can be proved by the disappearance of the absorption peak of the nitrile oxide group (2300 cm) by FT-IR analysis. Contact angle, TG-DTA and tensile-test experiments were conducted to characterize the wettability, thermo-stability and mechanical properties of the obtained cross-linked rubber materials, respectively. The results showed that the curing agent TTNO could cure PB at room temperature. With the growing content of the curing agent TTNO, the tensile strength of the obtained cross-linked rubber material increased by 260% and the contact angle increased from 75.29° to 89.44°. Moreover, the thermo-stability performances of the cross-linked rubber materials have proved to be very stable, even at a temperature of 300 °C, by TGA analysis.
作为复合固体推进剂的重要组成部分,交联链烯基聚合物需要在高温下固化,而目前的异氰酸酯固化体系对湿度高度敏感。本文提出了一种通过四甲基对苯二甲腈氧化物(TTNO)的腈氧化物与液体聚丁二烯(PB)的C=C基团进行环加成反应,对具有稳定润湿性的交联聚合物(聚丁二烯)进行低温固化的方法。TTNO由1,2,4,5-四甲基苯分四步合成,并被评估为用于固化液体PB的低温固化剂。为了表征TTNO在25℃下的反应能力,制备了固化剂TTNO含量不同(8%、10%、12%、14%、16%)的交联橡胶材料。通过傅里叶变换红外光谱(FT-IR)分析腈氧化物基团(2300 cm)吸收峰的消失,可以证明固化方法的可行性。分别进行了接触角、热重-差示热分析(TG-DTA)和拉伸试验,以表征所得交联橡胶材料的润湿性、热稳定性和力学性能。结果表明,固化剂TTNO可以在室温下固化PB。随着固化剂TTNO含量的增加,所得交联橡胶材料的拉伸强度提高了260%,接触角从75.29°增加到89.44°。此外,通过热重分析(TGA)可知,交联橡胶材料的热稳定性非常好,即使在300℃的温度下也是如此。