Department of Materials Engineering, Defence Institute of Advance Technology (DIAT), Pune 411025, India.
Fuel and Lubricant Division, Defence Materials and Stores Research & Development Establishment (DMSRDE), Kanpur 208013, India.
J Nanosci Nanotechnol. 2019 Dec 1;19(12):7982-7992. doi: 10.1166/jnn.2019.16870.
There are several chemical methods for the synthesis of high energy-density fuel, exotetrahydrodicyclopentadiene (exo-THDCPD), however, still there is a challenge to synthesize exo-THDCPD conveniently. In present work, the exo-THDCPD from dicyclopentadiene (DCPD) has successfully synthesized through simplest and greener single step hydroconversion reaction over mesoporous supported nickel nanocatalyst (Ni/MCM-41). The reaction performed in autoclave under a hydrogen pressure ranging from 300-400 (Psi), temperature range 130-150 °C and progress has been monitored by gas chromatography which reveals that the reaction mechanism goes through dissociation-recombination of DCPD. The major reaction parameters such as temperature, pressure and nanocatalyst have been experimentally examined for the yield (85%) of the product. The structural analysis of exo-THDCPD is carried out by H NMR and FTIR techniques and the physicochemical properties have also been evaluated. Good quality nanocatalyst Ni/MCM-41 has been synthesized by impregnation incipient wetness method and characterized by XRD, EDAX, TEM, and BET techniques. The nanocatalyst is highly reactive due to its mesoporous structure having appropriate size and shape which gives free diffusion of the molecules. Repeatability of the nanocatalyst shows good reactivity up to the four runs.
有几种化学方法可用于合成高能量密度燃料,例如四环戊二烯(exo-THDCPD),但仍存在方便合成 exo-THDCPD 的挑战。在本工作中,通过在介孔负载镍纳米催化剂(Ni/MCM-41)上进行最简单和最环保的一步加氢转化反应,成功地从二环戊二烯(DCPD)合成了 exo-THDCPD。反应在自生压力为 300-400(Psi)的高压釜中进行,温度范围为 130-150°C,并通过气相色谱进行监测,结果表明反应机理是通过 DCPD 的离解-重组进行的。主要反应参数,如温度、压力和纳米催化剂,已通过实验进行了考察,以获得 85%的产物收率。通过 H NMR 和 FTIR 技术对 exo-THDCPD 的结构进行了分析,并对其物理化学性质进行了评估。采用浸渍初始湿度法合成了高质量的介孔纳米催化剂 Ni/MCM-41,并通过 XRD、EDAX、TEM 和 BET 技术进行了表征。纳米催化剂具有介孔结构,尺寸和形状适当,可使分子自由扩散,因此具有高反应性。纳米催化剂的可重复性表明,其在四组运行中均具有良好的反应性。