CHARACTERIZATION AND GAS CHROMATOGRAPHY OF ALKOXIDES OF ALUMINUM AND OF SOME GROUP 4 ELEMENTS

Al-tris-isopropoxide, tetrakis-isopropoxides of Ti, Zr, Hf, Si and Ge, and tetrakis-tertiary amyloxides of Ti, Zr and Hf have been synthesized as precursor materials for the preparation of single and mixed phase refractory oxides. An attempt has been made to characterize these compounds on the basis of chemical analysis, infrared spectra, proton NMR, mass spectrometry, thermogravimetric analysis, and gas chromatography. The IR spectra (4000-270 cm-1) of the tetrakis-tertiary amyloxides of Ti, Zr, and Hf have been obtained for the first time. In the CsBr region a number of very strong absorption bands are found that are characteristic absorption frequencies for the tertiary amyl compounds. These compounds are liquid (with the exception of the Al compound which is solid), of considerable volatility, and thermally stable at relatively high temperatures when highly pure. Results of the gas chromatography of the above metal alkoxides are reported for the first time. Well resolved peaks have been obtained with a mixture of (i) t-amyloxides of Ti and Zr, (ii) t-amyloxides of Ti and Hf, (iii) isopropoxides of Si, Ge, Ti and Al. © 1969, American Chemical Society. All rights reserved.