FIELD: chemical industry.
SUBSTANCE: invention relates to a method for separating a mixture of erbium(III) bis(tetra-4-[2,4,5-trichlorophenoxy])phthalocyaninate and tetra-4-(2,4,5-trichlorophenoxy)phthalocyanine. The method is characterized by the sequential introduction of a reducing agent and an oxidizing agent into a chromatographic column, while before starting column chromatography on silica gel using chloroform as an eluent in a solution of a mixture of bis (tetra-4-[2,4,5-trichlorophenoxy]) erbium(III) phthalocyaninate and tetra-4-(2,4,5-trichlorophenoxy)phthalocyanine in chloroform, hydrazine hydrate is added as a reducing agent to convert the neutral radical form of erbium(III) bis(tetra-4-[2,4,5-trichlorophenoxy])phthalocyaninate ) into the restored form and incubated for at least 30 minutes. Restoration of the neutral-radical form is visually confirmed by a colour change from green to blue-blue, simplifying the visual control of the process. The resulting blue-blue solution is introduced into a chromatographic column, tetra-4-(2,4,5-trichlorophenoxy)phthalocyanine is isolated by elution with chloroform as a solution in chloroform, then the solvent is distilled, obtaining solid tetra-4-(2,4,5- trichlorophenoxy)phthalocyanine, while erbium(III) bis(tetra-4-[2,4,5-trichlorophenoxy])phthalocyaninate remaining at the start is in the reduced form. A solution of iron(III) acetylacetonate in chloroform is introduced into the chromatographic column to react with erbium(III) bis(tetra-4-[2,4,5-trichlorophenoxy])phthalocyaninate, forming a neutral radical form, which is visually confirmed by changing color from blue to green. Erbium(III) bis(tetra-4-[2,4,5-trichlorophenoxy])phthalocyaninate is isolated by elution with chloroform as a solution, then the solvent is distilled, obtaining solid bis(tetra-4-[2,4,5-trichlorophenoxy]) erbium(III) phthalocyaninate.
EFFECT: providing a method for the simplified and efficient separation of a mixture of bis(tetra-4-[2,4,5-trichlorophenoxy])erbium(III) phthalocyaninate and tetra-4-(2,4,5-trichlorophenoxy)phthalocyanine by column chromatography by using one solvent, which is also an eluent.
1 cl, 8 dwg, 1 ex
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Authors
Dates
2023-05-29—Published
2022-11-07—Filed