TY - JOUR
T1 - Effects of aluminum trichloride and magnesium chloride on the synthesis of ladder polyphenylsilsesquioxane
AU - Jiang, Yunyun
AU - Yang, Rongjie
PY - 2012
Y1 - 2012
N2 - Ladder polyphenylsilsesquioxane (Ph-LPSQ) has been synthesized at 80 °C through the hydrolysis and condensation of phenyltrichlorosilane (PhSiCl 3), with aluminum chloride (AlCl 3) or magnesium chloride (MgCl 2) 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 AlCl 3 and MgCl 2 on the structure regularity of Ph-LPSQ and the condensation polymerization have also been studied. The results showed that Ph-LPSQ could be obtained in the AlCl 3 and MgCl 2 systems, respectively, but the experimental phenomena and results showed significant differences between the two systems. SEM observation revealed spherical Ph-LPSQ particles from the PhSiCl 3/AlCl 3 system, but irregular and agglomerated Ph-LPSQ particles from the PhSiCl 3/1.5(MgCl 2) system. TGA, 29Si/NMR, and MALDI-TOF MS indicated that the ladder structure of Ph-LPSQ from the PhSiCl 3/1.5(MgCl 2) system was more regular. In the PhSiCl 3/AlCl 3 system, 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 AlCl 3 or MgCl 2 in the hydrolysis and condensation system favors the intermolecular condensation of intermediate products of polyhydroxyl silanol to form a regular ladder structure.
AB - Ladder polyphenylsilsesquioxane (Ph-LPSQ) has been synthesized at 80 °C through the hydrolysis and condensation of phenyltrichlorosilane (PhSiCl 3), with aluminum chloride (AlCl 3) or magnesium chloride (MgCl 2) 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 AlCl 3 and MgCl 2 on the structure regularity of Ph-LPSQ and the condensation polymerization have also been studied. The results showed that Ph-LPSQ could be obtained in the AlCl 3 and MgCl 2 systems, respectively, but the experimental phenomena and results showed significant differences between the two systems. SEM observation revealed spherical Ph-LPSQ particles from the PhSiCl 3/AlCl 3 system, but irregular and agglomerated Ph-LPSQ particles from the PhSiCl 3/1.5(MgCl 2) system. TGA, 29Si/NMR, and MALDI-TOF MS indicated that the ladder structure of Ph-LPSQ from the PhSiCl 3/1.5(MgCl 2) system was more regular. In the PhSiCl 3/AlCl 3 system, 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 AlCl 3 or MgCl 2 in the hydrolysis and condensation system favors the intermolecular condensation of intermediate products of polyhydroxyl silanol to form a regular ladder structure.
KW - Aluminum chloride
KW - Ladder structure
KW - Magnesium chloride
KW - Polyphenylsilsesquioxane
KW - Synthesis
UR - http://www.scopus.com/inward/record.url?scp=84867155607&partnerID=8YFLogxK
U2 - 10.2298/CICEQ110911018J
DO - 10.2298/CICEQ110911018J
M3 - Article
AN - SCOPUS:84867155607
SN - 1451-9372
VL - 18
SP - 421
EP - 430
JO - Chemical Industry and Chemical Engineering Quarterly
JF - Chemical Industry and Chemical Engineering Quarterly
IS - 3
ER -