A hybrid fluorescent pigment composed of fluorescent yellow X-10GFF (FY-10G) and palygorskite (PLG) was prepared by semi-dry grinding. The effects of the physically adsorbed water content and grinding time on the environmental stability of FY-10G/PLG hybrid fluorescent pigments in terms of acid, ethanol and ultraviolet irradiation are discussed in detail. The incorporated FY-10 G molecules are mainly trapped on the external surface and the groove of PLG. Due to the host–guest interaction between PAL and FY-10G, the emission spectrum of the FY-10G/PLG hybrids shifts to a greater wavelength compared with that of FY-10G, but the physically adsorbed water content and grinding time have no effect on the position of the emission spectrum except for its intensity. A larger, physically adsorbed water content and appropriate grinding time may effectively prevent the aggregation and breakage of the bundles of PLG and facilitate FY-10 G molecules to enter into the groove of PAL. This increases the environmental stability of the as-prepared hybrid pigments.