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Ladder polyphenylsilsesquioxane (Ph-LPSQ) has been synthesized at 80°C  through the hydrolysis and condensation of phenyltrichlorosilane (PhSiCl3),  with aluminum chloride (AlCl3) or magnesium chloride (MgCl2) as an assistant  reactant. The Ph-LPSQ obtained has been characterized and analyzed by SEM,  FTIR, TGA, 29Si NMR, and MALDI-TOF MS, and the effects of AlCl3and MgCl2on the  structure regularity of Ph-LPSQ and the condensation polymerizationhavealso  been studied. The results showed that Ph-LPSQ could be obtained in  theAlCl3and MgCl2systems, respectively, but the experimental phenomena and  results showed significant differences between the two systems. SEM observation  revealed spherical Ph-LPSQ particles from the PhSiCl3/AlCl3system, but  irregular and agglomerated Ph-LPSQ particles from the PhSiCl3/1.5(MgCl2)  system. TGA, 29SiNMR, and MALDI-TOF MS indicated that the ladder structure of  Ph-LPSQ from the PhSiCl3/1.5(MgCl2) system was more regular. Inthe  PhSiCl3/AlCl3system, Al could be incorporated into the ladder chain structure  through competing reactions between Si-O-Al and Si-O-Si, which slightly  decreased the regularity of the ladder chain structure of Ph-LPSQ. Mechanistic  analysis suggests that the presence of AlCl3or MgCl2in the hydrolysis and  condensation system favors the intermolecular condensation of intermediate  products of polyhydroxyl silanol to form a regular ladder structure

Effects of aluminum trichloride and magnesium chloride on the synthesis of ladder polyphenylsilsesquioxane