Preparation of MCM-41 incorporated with transition metal substituted polyoxometalate and its catalytic performance in esterification

The ordered mesoporous MCM-41 materials incorporated with transition metal substituted polyoxometalate (PW11O39M1)5− (designated as M1–POM, M1 = Ni2+, Co2+ or Cu2+) were synthesized via an original direct synthesis method. The samples were characterized by XRF, XRD, FT-IR, HRTEM, SEM and N2 adsorption isotherm techniques. The results show that M1–POM was uniformly dispersed in the samples and its structure remained intact in the materials. The samples exhibited excellent catalytic performance for the esterification of n-butanol with acetic acid, which is better than that of the supported lacunary polyoxometalate (PW11O39)7− and the impregnated (IM) samples.

The mesoporous MCM-41 materials were incorporated with transition metal substituted lacunary polyoxometalate by the direct synthesis method (DS) and the impregnation method (IM), respectively. Fig. A is 15%Ni–POM/MCM-41(DS), and Fig. B is 15%Ni–POM/MCM-41(IM).Figure optionsDownload as PowerPoint slideHighlights
► M1–POM was encapsulated into MCM-41 via an original direct synthesized method.
► The M1–POM/MCM-41 has well-ordered mesopores and spherical morphology.
► The M1–POM/MCM-41 samples showed good performance on the esterification.
► The strong interactions of M1–POM with the support ensured little loss of M1–POM.