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The single crystal Fe（acac）3 was successfully synthesized using acetylacetone and ferric oxide as the original materials. It was characterized by IR, UV-Vis, X-ray single crystal diffraction and TG-DSC. The results indicated that the crystal has an orthorhombic structure with space group Pbca and the crystallographic data of the complex are: a=1.5494（5）nm, b= 1.3595（5）nm, c=1.658 9（5）nm,α=β=γ=90o, V= 3.494（2） nm3, DC=1.343 (g·cm-3) , Z=8,μ=0.886 mm-1 , F（000） =1480. Fe（Ⅲ） ion is coordinated with six oxygen atoms from three Hacacs, and form a slightly distorted octahedron coordination geometry; The single crystal Zn（acac）2·H2O was successfully synthesized using acetylacetone and ferric oxide as the starting materials . It was tested by IR , UV-Vis , X-ray single crystal diffraction and TG-DSC. The result indicate that the crystal has an monoclinic structure with space group P21 and the crystallographic data of the complex are : a= 1.040 14（3） nm, b=0.537 620（10） nm, c=1.086 34（3） nm,α=90.00°,β=93.213（2）°,γ=90.00°, V=0.60653（3） nm3, DC=1.531 (g·cm-3), Z=2,μ=2.027 mm-1,F（000）=288. Acetylacetone negative ion is coordinated with Zn（Ⅱ） ion in the form of olefine alcohol ion. Zn（Ⅱ） of the complextion is at the central of the slightly metamorphotic tetragonal pyramid.TAC-Fe（acac）3 as initiators, to trigger the emulsion polymerization of MMA, the influence on the amount of initiator, reaction time, polymerization temperature of MMA conversion in the reaction system was studied. The optimum reaction condition was as follows: Fe（acac）3 dosage=0.3% of the amount of monomer; reaction time 5h; polymerization temperature at 70℃; flow rate of nitrogen at 80ml/min.Fe（acac）3, Zn（acac）2·H2O as the main raw materials, prepared precursor with even particle by homogeneous precipitation method, and then direct calcination to prepare ZnFe2O4 nanocrystalline materials. XRD showed that the iron zinc phase of grain was formed in the precursor, but grain development is not yet complete, and must contain amorphous components. ZnFe2O4 materials with the crystal of more fully transformation was prepared by calcining precursor. TEM showed that the precursor was the spherical particles and narrow particle size distribution. Each spherical particle was formed by many of the small particles. Nano-ZnFe2O4/PMMA composite materials was prepared by in situ emulsion polymerization of MMA. TEM showed that the latex particle in the solution were spherical and possessed good dispersing in the synthesis system, and the composite particles had a clear core shell structure.
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