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D.L-Mandelato Zirconium(Ⅳ) Complex의 物理的 特性과 加熱條件에 따른 構造變化
丁梧鎭,조경호,문경찬 조선대학교 기초과학연구소 1983 自然科學硏究 Vol.6 No.1
The dl-monomandelate zirconium(Ⅳ) and dl-tetramandelato zirconium(Ⅳ) complexes were synthesized from ZrOCl_2, 8H_2O and it was identified by UV-spectrum, IR-spectrum and element analysis, respectively. These transitional state and determination of structures according to heating curves were identified by aalytical methods of electron microphotograp and X-ray diffractiometry. The results obtained are as follows: 1) The dl-monomandelato zirconium(Ⅳ) complex obtained from the result of elements analysis for complexes synthesized was analyzed; H=3.60%, C=37.66% and Zr=31.03%. respectively and the dl-tetramandelato zirconium(Ⅳ) complex; H=4.153% C=55.23% and Zr=13.09%, respectively. 2) The dl-tetramandelato zirconium(Ⅳ) complexes were appeared with symmetric carbonyl streching mode from 1500 to 1700㎝^-1 and this symmetric carbonyl streching mode means the presense of coordinate bonding between Zr and carboxylic radical. 3) The mode of dl-monomandelato zirconium(Ⅳ) complex has asymmetrical peak, and this means the state for coordinate bonding of Zr-coo-but dl-tetramandelato zirconium(Ⅳ) complexes have symmetric peak in the range of 1000 to 1500㎝^-1 and this peak means the presence of more than one kind of zirconium carboxyl bond. 4) The dl-mono and tetramandelato zirconium(Ⅳ) complexes are formed in rtrong absorption band at 1360㎝^-1, and this values are shifted with respect to 1385㎝^-1 of the dl-mandelic acid, and complex compound synthesized from state of acetonitrile solution, is formed with strong carboxyl(vsy) band of absorption at 1360㎝^-1 and 1650㎝^-1, respectively. 5) The vcoo(sy) band of absorption at 1360~1385㎝^-1 range means to be eight coordinate complex and frequency of this range have vcoo characterics of structure. The weak band of absorption of the 2700㎝^-1 show the structure of coordinate bonding and this band have the typical harmonic vibration structure of O-H-O bonding. 6) The dl-mandelato zirconium(Ⅳ) complex in NH_4OH solution exhibits the maximum absorbany at 255mm. The maximum molar absorptivity of^-4 M dl-mono and tetramandelato zirconium(Ⅳ) complex have 0.54×10^4 and 1.2×10^4, respectively. 7) The white products (synthetic complex) precipitated from aqueous solution is polymeric with hydrogen bonding and this complexes are also insoluble in organic solvent as C_6H_6, C_2H_5OH, DMSO, and CH_3OHㆍㆍㆍetc. but is soluble in NH_4OH 8) The dl-mono and tetramandelato zirconium(Ⅳ) complex exhibit the endothermic peak of dehydration at 218.75℃ and 209.4℃, respectively. and exhibit the exothermic peak of decomposition for H_2O and CO at below 600℃ and 1050℃ in air calcination, respectively. 9) The synthetic complexes are formed with exothermic peaks transed from ZrO_2-monoclinic system to ZrO_2-tetragonal system at 1250℃ in air calcination. 10) The synthetic complexes have amorphous at below 110℃, and are appeared with ZrO_2-monoclinic systems in air calcination, respectively. If synthetic complexes are heated at 970℃ and 110℃ in air calcination, respectively. The clear crystalline structures of ZrO_2-monoclinic system are identified by X-ray diffractiometry and analytical method of electron microscope. and intensities of X-ray diffraction patterns are increased more trikis complex compound than mono complex.
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