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Preparation of P(MBA‐ co ‐MAA)/Zr(OH) 4 /P(EGDMA‐ co ‐MAA)/TiO 2 Tetra‐layer Hybrid Microspheres and the Corresponding ZrO 2 /TiO 2 Double‐shelled Hollow Microspheres
Author(s) -
Qin Dianbin,
Yu Jinhui,
Bian Guomin,
Qi Yonglin,
Zhang Dongwei,
Yang Xinlin
Publication year - 2014
Publication title -
chinese journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.28
H-Index - 41
eISSN - 1614-7065
pISSN - 1001-604X
DOI - 10.1002/cjoc.201300676
Subject(s) - methacrylic acid , chemistry , zirconium , copolymer , polymer chemistry , nuclear chemistry , calcination , cubic zirconia , polymer , chemical engineering , inorganic chemistry , organic chemistry , catalysis , ceramic , engineering
Double‐shelled zirconia/titania (ZrO 2 /TiO 2 ) hollow microspheres were prepared by the selective removal of the polymer components via the calcination of the corresponding tetra‐layer poly( N , N′ ‐methylenebisacryl amide‐ co ‐methacrylic acid) (P(MBA‐ co ‐MAA))/Zr(OH) 4 /poly(ethyleneglycol dimethacrylate‐ co ‐methacrylic acid) (P(EGDMA‐ co ‐MAA))/TiO 2 hybrid microspheres. These tetra‐layer microspheres were synthesized by the combination of the distillation copolymerization of N , N (‐methylenebisacryl amide‐ co ‐methacrylic acid (MBA) or ethyleneglycol dimethacrylate (EGDMA) crosslinker and methacrylic acid (MAA) for the preparation of polymer core and third‐layer as well as the controlled sol‐gel hydrolysis of inorganic precursors for the construction of zirconium hydroxide (Zr(OH) 4 ) and titania (TiO 2 ) layers. The thicknesses of zirconia and titania shell‐layers were conveniently controlled via varying the feed of zirconium n ‐butoxide (Zr(OBu) 4 ) and titanium tetrabutoxide (TBOT) during the sol‐gel hydrolysis, while the sizes of polymer layers were tuned through a multi‐stage distillation precipitation copolymerization. The structure and morphology of the resultant microspheres were characterized by transmission electron microscopy (TEM), X‐ray diffractometer (XRD), X‐ray photoelectronic spectroscopy (XPS), and thermogrametric analysis (TGA).