Titanium ethoxide is prepared by treating titanium tetrachloride with ethanol in the presence of an amine: The purity of titanium ethoxide is commonly assayed by proton NMR spectroscopy. Ti41H NMR : 4.36, 1.27.
Structure
Both Ti4 exist mainly as tetramers with an octahedral coordination environment around the metal centers. There are two types of titanium centers, depending on the number of terminal vs bridging alkoxide ligands. Zr4 is structurally similar. The virtual symmetry of the M4O16 core structure for the tetramer structures of these compounds is C2h.
Related compounds
Titanium methoxide
Like the ethoxide, titanium methoxide Ti4 exists as a tetramer with each of the TiIV metal centers having an octahedral coordination environment.
Titanium isopropoxide
With bulky alky groups, Ti4 in contrast exist as a monomer with a tetrahedral environment around the Ti center. This lowerdegree of coordination to the metal center is attributed to the steric bulk of the iPr groups versus the n-alkyl groups, this serves to prevent bridging interactions between the metal centers.
Zirconium ethoxide
Zirconium ethoxide can be prepared in a manner similar but not identical to the titanium compound: A more common synthesis for zirconium ethoxide is to treat zirconium tetrachloride with the desired alcohol and ammonia: Zirconium ethoxide can also be prepared with zirconocene dichloride:
Zirconium propoxide
Zr4 also adopts the titanium ethoxide structure.
Reactions
Both Ti and Zr alkoxides can be used to deposit microstructured films of TiO2 or ZrO2: These films form via a hydrolysis of the alkoxide at a surface interface. It is important to note that the TiO2 and ZrO2 formed by these reactions have a polymeric structure which is where their utility as waterproofing, scratch resistant or heat resistant coatings comes from. The structure of the metal oxide films grown in this matter is affected by the presence of base or acid catalysts for the hydrolysis. Generally acid-catalysis yields a sol where the polymer chains are randomly oriented and linear. In the base-mediated case bushy clusters or crosslinked networks are produced, these structures can trap solvent and reaction byproducts and form a gel coating. TiIV and ZrIV alkoxides are also potential starting materials for Ziegler–Natta catalysts used in alkene polymerization.