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Synthesis of SAPO-16 molecular sieve in non-aqueous medium by microwave method using Hexamethyleneimine as a template
Microporous and Mesoporous Materials ( IF 4.8 ) Pub Date : 2017-12-11 , DOI: 10.1016/j.micromeso.2017.12.008
Siliveri Suresh , Ingala Ajit Kumar Reddy , Narayanan Venkatathri

An Aluminophosphate with sequence number Six Teen (AST) type framework silico alumino phosphate (SAPO-16) molecular sieve is successfully synthesized through an eco-friendly, economic and a faster crystallization method by microwave treatment. In the present investigation, SAPO-16 is synthesized in a non-aqueous medium using hexamethyleneimine as a template. The structural and morphological properties are characterized by PXRD, SEM-EDX, TEM, BET, FT-IR, NH3-TPD, and MAS-NMR techniques. Powder X-ray diffraction studies show that the synthesized samples are highly crystalline. EDX results showed that the calcined sample contains 0.7 Al2O3: 0.8 P2O5: 0.4 SiO2 on the surface. TEM analysis inferred that the sample contains 50-100 nm sized particles with uniformed triangle morphology. The TGA analysis reveals that the sample loses about 20% of it's weight from room temperature to 550 °C. BET-adsorption isotherm shows that the surface area is 270 m2/g. Structural integrity is shown by FT-IR analysis and Magic angle spinning Nuclear magnetic resonance spectroscopic analysis. 29Si MAS NMR analysis infers that most of the Si is present in tetrahedral Si:2Al:2Si environment. TPD-NH3 reveals that the presence of maximum amount of strong Brønsted acidity with minor amount of moderate bronsted acidity. The catalytic activity on Benzaldehyde acetalization reaction shows that the reactants have a maximum of 80% conversion in 8 h with maximum turn over a number of 14.5 × 10−2 and turn over the frequency of 4.0 × 10−5.



中文翻译:

六亚甲基亚胺为模板的微波法在非水介质中合成SAPO-16分子筛

通过生态友好,经济,快速的结晶方法,通过微波处理成功地合成了序列号为六个青少年(AST)型骨架硅铝磷酸盐(SAPO-16)的铝磷酸盐。在本研究中,SAPO-16是在非水介质中以六亚甲基亚胺为模板合成的。通过PXRD,SEM-EDX,TEM,BET,FT-IR,NH 3 -TPD和MAS-NMR技术表征结构和形态特性。粉末X射线衍射研究表明,合成的样品是高度结晶的。EDX结果表明,煅烧后的样品中含有0.7 Al 2 O 3:0.8 P 2 O 5:0.4 SiO 2。在表面上。TEM分析推断该样品包含50-100 nm大小的颗粒,具有均匀的三角形形态。TGA分析表明,从室温到550°C,样品的重量减少了约20%。BET吸附等温线表明表面积为270m 2 / g。FT-IR分析和魔角旋转核磁共振光谱分析显示了结构的完整性。29 Si MAS NMR分析表明,大多数Si存在于四面体Si:2Al:2Si环境中。TPD-NH 3表明存在最大量的强布朗斯台德酸度和少量的中等布朗斯台德酸度。苯甲醛缩醛化反应的催化活性表明,反应物在8 h内具有最高80%的转化率,最大转化数为14.5×10 -2,翻转频率为4.0×10 -5

更新日期:2017-12-11
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