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To explore the simple preparation method of glycerol metal chelates and effectively expand the application field of glycerol metal chelates and biomass glycerol, the micro‐nanopowders such as glycerin zinc (Gly‐Zn), and glycerin bismuth (Gly‐Bi) were prepared by the solid‐phase reaction, using sodium benzene sulfonate as a catalyst and template. Theoretical calculation of deprotonation reaction energy of glycerol and zinc chloride, bismuth nitrate was performed with the framework of DFT, and their structures were characterized by X‐ray diffraction, Fourier‐transform infrared spectroscopy (FTIR), scanning electron microscope and X‐ray photoelectron spectroscopy. The thermal stability of Gly‐Zn and Gly‐Bi for polyvinyl chloride (PVC) is discussed by TG. The results show that the deprotonation reaction of glycerol with zinc chloride or bismuth nitrate mainly occurs in the dehydrogen of secondary hydroxyl (OsecH) and primary hydroxyl (OprimH) of glycerol molecules, and the H of OsecH is more active than that of the OprimH. The obtained Gly‐Zn and Gly‐Bi have good micromorphology with the rod‐like and bar‐like respectively. Applied them as thermal stabilizers to PVC processing, the reaction kinetic constant (k, s−1) is an order of kPVC > kPVC/Gly‐Zn > kPVC/Gly‐Bi. After the additions of 10% Gly‐Zn and 10% Gly‐Bi, the thermal stability time (min) of PVC, PVC/Gly‐Zn and PVC/Gly‐Bi is 45, 54.43 and 71.47, respectively. [ABSTRACT FROM AUTHOR]