Nickel–Sodalite: An Efficient Catalyst for Selective Hydrogenation of Dicyclopentadiene

IF 2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY
Azeem Khan, Ankit Mishra, Vikas Verma, Saleem Akhtar Farooqui, Anil Kumar Sinha
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Abstract

In the current study, the hydrogenation of dicyclopentadiene (DCPD) to endo-tetrahydrodicyclopentadiene (endo-THDCPD) is performed using a sodalite-supported nickel (Ni–SOD) catalyst. The synthesized catalyst was characterized using various characterization techniques including temperature-programmed reduction (TPR), ammonia temperature-programmed desorption (NH3-TPD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FT-IR). The total acidity as determined via TPD and Ni crystallite size as determined via PXRD were 0.22 mmol/gcat and 7.8 nm, respectively. The reaction parameters were optimized using the Ni–SOD catalyst (4 wt% Ni) for the hydrogenation of DCPD. A low Ni content of 4 wt% was required to achieve complete conversion and >99% selectivity. The optimized reaction parameters were 90 °C, 10 bar hydrogen pressure, 800 RPM stirring rate, catalyst: feed ratio of 0.1, and 6 h reaction time. This is the first report of the low-temperature activity of the Ni catalyst under solvent-free conditions, which removes all the possibility of side reactions such as retro-Diels–Alder reaction (RDAR). The yield of the hydrogenation reaction product, endo-THDCPD, was 99.5% using the Ni–SOD catalyst.

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镍-钠盐:选择性加氢二环戊二烯的高效催化剂
在本研究中,使用钠盐负载镍(Ni-SOD)催化剂将双环戊二烯(DCPD)加氢为内-四氢双环戊二烯(内- thdcpd)。采用程序升温还原(TPR)、氨程序升温脱附(NH3-TPD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、粉末x射线衍射(PXRD)、x射线光电子能谱(XPS)、热重分析(TGA)和傅里叶变换红外光谱(FT-IR)等表征技术对合成的催化剂进行了表征。TPD法测定的总酸度为0.22 mmol/gcat, PXRD法测定的Ni晶粒尺寸为7.8 nm。以Ni - sod (4 wt% Ni)为催化剂,优化了DCPD加氢的反应参数。要实现完全转化和99%的选择性,需要低镍含量为4 wt%。优化后的反应参数为:温度90℃,氢气压力10 bar,搅拌速度800 RPM,催化剂与进料比0.1,反应时间6 h。这是第一次报道镍催化剂在无溶剂条件下的低温活性,消除了所有副反应的可能性,如反diels - alder反应(RDAR)。在Ni-SOD催化剂的催化下,加氢产物thdcpd的产率为99.5%。
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来源期刊
ChemistrySelect
ChemistrySelect Chemistry-General Chemistry
CiteScore
3.30
自引率
4.80%
发文量
1809
审稿时长
1.6 months
期刊介绍: ChemistrySelect is the latest journal from ChemPubSoc Europe and Wiley-VCH. It offers researchers a quality society-owned journal in which to publish their work in all areas of chemistry. Manuscripts are evaluated by active researchers to ensure they add meaningfully to the scientific literature, and those accepted are processed quickly to ensure rapid online publication.
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