Реакция #470356

Уравнение реакции

sodium

o-phthalonitrile

sodium

→

phthalocyanine

Растворители

acetone

Условия реакции

Обработка

1. 1
   Другоеwas prepared
2. 2
   Другоеwas prepared
3. 3
   Другоеto yield NaX
4. 4
   Другоеa volatile component was removed from the react ion mixture
5. 5
   Другоеto give a solid
6. 6
   ДругоеThe solid was purified through extraction sequentially with methanol, acetone, and pyridine in a Soxhlet extractor
7. 7
   Другоеto remove unnecessary substances such as unreacted ligand

Методика

A zeolite X powder including Co2+-phthalocyanine complex (CoPc) was prepared according to the following procedure. Specifically, a powder (product supplied by Tosoh Corporation) of zeolite X containing sodium ions (NaX) was prepared, and part of sodium ions (Na+) contained in the zeolite were exchanged with cobalt ions (Co2+) through ion exchange to yield NaX containing 0.95 percent by weight of Co2+ ions (Co—NaX). In acetone were stirred 108.96 g of the Co—NaX (containing 18 mmol of Co2+) and 0.127 mol of o-phthalonitrile for one hour, a volatile component was removed from the react ion mixture, and the residue was suspended in 250 mL of ethylene glycol. The suspension was combined with 15 mL of tri-n-butylamine ((n-Bu)3N), and the mixture was stirred at 210° C. for 5 hours to give a solid. The solid was purified through extraction sequentially with methanol, acetone, and pyridine in a Soxhlet extractor to remove unnecessary substances such as unreacted ligand contained in the solid and phthalocyanine that had formed outside the zeolite pores. The purified product was suspended in 400 mL of a saturated aqueous solution of sodium nitrate, followed by stirring for 24 hours, to remove unreacted cobalt ions that had remained without forming the complex through exchange with sodium ions. The resulting substance was washed with water, dried at 60° C., and thereby yielded a pale blue powder. The energy dispersive X-ray spectroscopy (EDX), ultraviolet-visible (UV/vis) absorption spectra, and diffuse reflection spectra of the powder verified that a target substance (CoPc@NaX) composed of NaX and cobalt phthalocyanine encapsulated in the NaX unit cell was obtained.

Источник