Method for producing redox-active Ti(IV) coordination compounds
View Patent ↗A method for producing an aqueous solution of a redox-active coordination compound of a transition metal which can be used directly as an electrolyte in a flow battery wherein the method comprises reacting a freshly precipitated hydrous transition metal oxide with a chelating agent and a base in an aqueous reaction medium to produce a solution of the corresponding redox-active transition metal coordination compound.
1. A method for producing a redox-active coordination compound of a transition metal selected from the group consisting essentially of titanium, aluminum, chromium, iron, vanadium, manganese, cerium, and uranium which comprises:
(a) precipitating a soluble salt of the transition metal with a base in an aqueous reaction medium to form freshly precipitated hydrous transition metal oxide;
(b) separating the freshly precipitated hydrous transition metal oxide from the aqueous reaction medium; and
(c) reacting the freshly precipitated hydrous transition metal oxide with a chelating agent and a base in a second aqueous reaction medium to produce a solution of the corresponding redox-active transition metal coordination compound.
2. The method of claim 1 wherein the redox-active coordination compound is Ti(IV) and the method comprises:
(a) precipitating a soluble titanium salt with a base in an aqueous reaction medium to form freshly precipitated hydrous titanium oxide;
(b) separating the freshly precipitated hydrous titanium oxide from the aqueous reaction medium; and
(c) reacting the freshly precipitated hydrous titanium oxide with a chelating agent and a base in a second aqueous reaction medium to produce a solution of the corresponding redox-active Ti(IV) coordination compound.
3. The method of claim 2 wherein the freshly precipitated hydrous titanium oxide in step (b) is separated by filtration and washing with water.
4. The method of claim 2 which includes the additional steps of:
(d) crystallizing the corresponding Ti(IV) coordination compound to form a crystalline solid; and
(e) separating the crystalline solid from the aqueous solution.
5. The method of claim 2 wherein the soluble titanium salt in step (a) is selected from TiOCl 2 and TiOSO 4 , and the base in step (a) is selected from NaOH, KOH, and NH 4 OH.
6. A method for producing a Ti(IV) redox-active coordination compound which comprises:
(a) precipitating a metalloorganic compound of titanium with water to form freshly precipitated hydrous titanium oxide;
(b) separating the freshly precipitated hydrous titanium oxide from the aqueous reaction medium; and
(c) reacting the freshly precipitated hydrous titanium oxide with a chelating agent and a base in a second aqueous reaction medium to produce a solution of the corresponding redox-active Ti(IV) coordination compound.
7. The method of claim 6 wherein the metalloorganic compound of titanium is selected from the group consisting essentially of titanium tetraisopropoxide, titanium tetra-n-propoxide, titanium tetra-n-butoxide, titanium tetraethoxide, and titanium tetramethoxide.