Process for the preparation of metal diphthalocyanines

Chemistry of carbon compounds – Miscellaneous organic carbon compounds – C-metal

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26024586, C09B 4704

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active

043338763

ABSTRACT:
The diphthalocyanines of certain tri- and tetravalent metals, especially those of the empirical general formulae (PC).sub.2 H.M.sup.III (Ia) or (PC).sub.2. M.sup.IV (Ib) (wherein M.sup.III and M.sup.IV represent respectively the tri- and tetravalent metal, and "PC" represents the phthalocyanine ring system) are well-known for their semiconductor and/or electrochromic properties. They are presently prepared by a process in which an organic derivative of the metal (an acetate, for example) is reacted, at about 300.degree. C. in a sealed tube, with an appropriate phthalonitrile. This process is itself unsatisfactory, and the invention provides a novel preparative process, process technique and application method. Thus, the inventive process involves reacting the metal (in the form of a complex with a 2,4-diketone, preferably acetyl acetone) with a large (about 100%) molar excess (based on the metal) of the phthalocyanine (preferably phthalocyanine itself) to give the desired diphthalocyanine, while the inventive technique places the reagents together as two layers in contact, the phthalocyanine layer being above the metal diketone complex layer, and slowly heats the whole to a temperature above that at which the diketone complex vaporizes. The inventive method prepares the metal diphthalocyanine using the inventive process and technique, and places the surface upon which the compound is to be deposited within the reaction vessel adjacent the reagents so that the formed diphthalocyanine is condensed directly thereon.

REFERENCES:
patent: 3027391 (1962-03-01), Frigerio
Moser et al., Phthalocyanine Compounds, pp. 104 to 107, 125-127, Reinhold Publishing Corp., NY. (1963).

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