Accelerated synthesis of Sn-BEA in fluoride media: effect of H2O content in the gel

作者：Yakimov Alexander V; Kolyagin Yury G; Tolborg Soren; Vennestrom Peter N R; Ivanova Irina I

来源：New Journal of Chemistry, 2016, 40(5): 4367-4374.

DOI：10.1039/c6nj00394j

Tin-containing zeotypes, particularly Sn-BEA, are promising heterogeneous catalysts for a number of important industrially relevant reactions. However, the direct hydrothermal synthesis of these materials requires unfavourably long times, which is an obstacle for their industrial application. In the present study we show that up to 4-fold reduction of the crystallization time can be achieved by a decrease of the H2O/SiO2 ratio in the synthesis gel from 7.5 to 5.6. The crystallization kinetics has been studied for five series of gels containing 1.0SiO(2) : 0.27TEA(2)O: xSnO(2) : 0.54HF : yH(2)O, for which y was fixed to 5.6, 6.8 and 7.5 at x = 0.005 and to 5.6 and 6.8 at x = 0.010. The crystallization time was varied within 0.5-60 days. The intermediate and final products obtained were investigated using XRD, FTIR, XRF, SEM, UV-Vis, MAS NMR spectroscopy and nitrogen adsorption-desorption techniques. The products obtained with lower water content are shown to have the same structure, textural properties and morphology as materials synthesized with higher water content. Although the size of the crystals is found to decrease with water content in the gel, it does not affect the Sn coordination and environment as confirmed by Sn-119 MAS NMR.

• 出版日期2016