Synthesis and characterization of pure ZnO and ZnO supported MgF2 for catalytic acylation of phenol

IF 1.7 4区 化学 Q3 CHEMISTRY, INORGANIC & NUCLEAR
Ika Fitri Ulfindrayani, Irmina Kris Murwani, Eko Sri Kunarti, Afifah Rosyidah, Harsasi Setyawati, Qurrota A’yuni, Abdul Wafi, Eka Cahya Muliawati
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Abstract

The catalysts MgF2 supported ZnO (0; 2.5; 5; 7.5; 10 and 15% w/w) were synthesized by sol-gel method. The structure of the catalysts were characterized by XRD. The acidity of the catalyst determined by pyridine-FTIR method showed that 7.5% ZnO/MgF2 had the highest acidity. The surface area of the ZnO/MgF2 was measured by N2 adsorption-desorption method. The surface area of the ZnO/MgF2 catalysts decrease with the increase in Zn content. The measurement SBET of the catalysts was in range of 5.31 to 9.44 m2/g. The morphology of the catalyst was observed by Scanning Electron Microscope (SEM). The synthesized catalysts performance was tested in phenol acylation and were determined by High Performance Liquid Chromatography (HPLC), which the main products were p-HAP (hydroxyacetophenone) and PA (phenyl acetate). The formation of p-HAP was influenced by the Lewis acid site, while PA was influenced by the Brønsted acid site. The highest conversion was achieved 85.36% by 7.5% ZnO/MgF2, while the yields of the p-HAP and PA were 56.06 and 23.40% respectively.

Abstract Image

纯氧化锌及氧化锌负载MgF2催化苯酚酰化反应的合成与表征
采用溶胶-凝胶法制备了MgF2负载ZnO(0、2.5、5、7.5、10和15% w/w)的催化剂。用XRD对催化剂的结构进行了表征。吡啶-红外光谱法测定了催化剂的酸度,结果表明7.5% ZnO/MgF2的酸度最高。采用N2吸附-解吸法测定ZnO/MgF2的表面积。ZnO/MgF2催化剂的比表面积随Zn含量的增加而减小。催化剂的SBET测量范围为5.31 ~ 9.44 m2/g。用扫描电镜(SEM)观察了催化剂的形貌。对合成的催化剂在苯酚酰化反应中的性能进行了测试,并采用高效液相色谱法对其进行了测定,主要产物为p-HAP(羟基苯乙酮)和PA(乙酸苯酯)。p-HAP的形成受Lewis酸位的影响,而PA的形成受Brønsted酸位的影响。7.5% ZnO/MgF2的转化率最高,达到85.36%,p-HAP和PA的收率分别为56.06和23.40%。
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来源期刊
Transition Metal Chemistry
Transition Metal Chemistry 化学-无机化学与核化学
CiteScore
3.60
自引率
0.00%
发文量
32
审稿时长
1.3 months
期刊介绍: Transition Metal Chemistry is an international journal designed to deal with all aspects of the subject embodied in the title: the preparation of transition metal-based molecular compounds of all kinds (including complexes of the Group 12 elements), their structural, physical, kinetic, catalytic and biological properties, their use in chemical synthesis as well as their application in the widest context, their role in naturally occurring systems etc. Manuscripts submitted to the journal should be of broad appeal to the readership and for this reason, papers which are confined to more specialised studies such as the measurement of solution phase equilibria or thermal decomposition studies, or papers which include extensive material on f-block elements, or papers dealing with non-molecular materials, will not normally be considered for publication. Work describing new ligands or coordination geometries must provide sufficient evidence for the confident assignment of structural formulae; this will usually take the form of one or more X-ray crystal structures.
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