反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 210 °C
PROCEDURE
实验过程
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.
WORKUP
后处理
- customwas prepared
- customwas prepared
- customto yield NaX
- customa volatile component was removed from the react ion mixture
- customto give a solid
- customThe solid was purified through extraction sequentially with methanol, acetone, and pyridine in a Soxhlet extractor
- customto remove unnecessary substances such as unreacted ligand