D. Nurpeisova, A. Тashenov, Z. Jakupova, S. Dosmagambetova, L. Omarova
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引用次数: 0
Abstract
A modified method for the synthesis of metallooctachlorophthalocyaninesand methods for their purification based on their sequential treatment with hydrochloric acid (10%) sodium hydroxide (2M), then again with hydrochloric acid (10%), pyridine (O.S.C.) in 1,2,4-trichlorobenzene as a solvent is presented. As a result, the degree of purification of copper ion complexes was achieved, 99% versus the best result using methods known in the literature 93%, for cobalt the degree of purity was 98% versus 88%. The yield of the products is also higher than in the known methods and amounted to 78, cobalt -43 for copper compounds. Physico-chemical methods have established that after the final stage of purification-pyridine treatment, impurities are removed, including cyanuric acid, the decomposition product of urea, the results of elemental analysis for carbon, hydrogen, nitrogen conducted on the ThermovomTypFlashEA 1112 analyzer complexes of cobalt (II), copper (II) with phthalocyanine, the assignment of bands of IR spectra recorded in KBr tablets on the Nicolet IR-200 FT -IR spectrophotometer, UV-the spectra of sulfuric acid solutions of metallooctachlorophthalocyanines taken on a Varian, UV -Vis/NIR spectrometer.
本文提出了一种改进的金属环氯酞菁的合成方法和以1,2,4-三氯苯为溶剂,先用盐酸(10%)、氢氧化钠(2M),再用盐酸(10%)、吡啶(o.s.c)进行顺序处理的纯化方法。结果,铜离子配合物的纯度达到了99%,而文献中已知的最佳纯度为93%,钴的纯度为98%,而文献中已知的纯度为88%。产物的收率也高于已知方法,铜化合物的收率为78,钴-43。理化方法证实,经过最后阶段的纯化-吡啶处理后,杂质被去除,包括氰脲酸,尿素的分解产物,在ThermovomTypFlashEA 1112分析仪上对钴(II)、铜(II)与酞菁配合物进行碳、氢、氮元素分析的结果,在Nicolet IR-200 FT -IR分光光度计上记录的KBr片的红外光谱谱带分配。用瓦里安紫外-可见/近红外光谱仪测定硫酸溶液中金属氯酞菁的紫外光谱。