INTERCALATION OF COBALT PHTHALOCYANINE INTO THE LAYERED HOST MATERIAL ANTIMONY HYDROGEN PHOSPHATE HSB(PO4)2 - IN-SITU SYNTHESIS OF GUEST MOLECULES

Cobalt phthalocyanine (CoPc) has been prepared in situ as a guest molecule in the layered host antimony hydrogen phosphate, which has also been called a phosphatoantimonic acid, HSb(PO4)2, here denoted as (HSbP2). The 8% cobalt exchanged HSbP2 was heated with molten 1,2-dicyanobenzene (DCB) at 230-240-degrees-C for periods between one and four hours. FTIR and UV-vis spectra indicate that the principal in situ reaction took place between three and four hours. The powder XRD data indicated that there was only a small increase (2.3 angstrom) in the interlayer spacing on formation of the CoPc molecule which, therefore, lies between the layers with the Pc rings parallel to the planes of the phosphate layers of the host. Changes in the FTIR spectra and in the P-31 MAS NMR spectra of the host suggest that the phthalocyanine ring interacts only weakly with the phosphate groups. Two different types of phosphorus atoms were identified in the solid state MAS NMR. The strong peak at - 20.82 ppm was assigned to the P in the undissociated POH group which was covered by the CoPc guest molecules. The weaker peak at + 4.92 ppm was assigned to the dissociated PO-H+ group which arose from the formation of a small amount of H2Pc and proton transfer to the ring nitrogen atoms. The hexagonal platelet crystal habit of the host is quite different from the acicular habit of the intercalation product. There was, however, no evidence for delamination followed by reformation of the layers during the synthesis.