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1 引言 整合纤维素制备工艺简单,性能优越,成本低廉,因而在分离集中已获得日趋增多的应用。本文将氨基硫脲基团接枝于棉纤维上,合成了氨基硫脲新型螫合纤维素(以下简称CC-TSC),并结合原子吸收测定,考察了CC-TSC柱法分离富集钯的最佳条件。结果表明,CC-TSC用于痕量钯的分离富集具有上柱速度快,易于解脱,富集倍数大,且选择性好,允许共存离子量大等优点。 2 实验部分 2.1 仪器与试剂 WFX-1E原子吸收分光光度计;钯空心阴极灯;仪器工作条件为:灯电流2mA,波长244.8nm,燃烧器高度6mm,狭缝宽度0.1mm,乙炔流量0.9L/min,空气流量6.5L/min,钯标准溶液1mg/ml(储备液):其它试剂均为分析纯级。 2.2 CC-TSC-的合成 在装有搅拌器,温度计及回流冷凝管的三口烧瓶中,加入环氧丙烷6ml,乙醇1ml,高氯酸0.12ml,水0.6ml,用甲苯稀释至60ml,充分搅拌。加入经20％NaOH溶液处理好的干燥棉纤维2g,恒温水浴加热控制温度为90～95℃。回流反应4h,抽滤,洗涤,65℃烘干即得中间产品2-氯-2-羟基丙基纤维素醚(CHPC)。
1 Introduction Integrated cellulose preparation process is simple, superior performance, low cost, and thus has been increasingly concentrated in the separation of applications. In this paper, thiosemicarbazone groups were grafted onto cotton fibers, and thiosemicarbazone (CC-TSC) was synthesized. The contents of palladium were determined by CC-TSC column with atomic absorption spectrometry Optimal conditions. The results show that CC-TSC can be used for the separation and enrichment of trace amounts of palladium with the advantages of high column speed, easy release, large enrichment factor, good selectivity and large amount of co-existing ions. 2 Experimental 2.1 Instruments and reagents WFX-1E atomic absorption spectrophotometer; palladium hollow cathode lamp; instrument operating conditions: lamp current 2mA, wavelength 244.8nm, burner height 6mm, slit width 0.1mm, acetylene flow 0.9L / min, air flow 6.5L / min, palladium standard solution 1mg / ml (stock solution): Other reagents are of analytical grade. 2.2 Synthesis of CC-TSC- A three-necked flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 6 ml of propylene oxide, 1 ml of ethanol, 0.12 ml of perchloric acid and 0.6 ml of water, and the mixture was diluted with toluene to 60 ml and stirred well . Adding 20% NaOH solution treated dried cotton fiber 2g, constant temperature water bath heating control temperature of 90 ~ 95 ℃. Reflux reaction 4h, suction filtration, washing, drying at 65 ℃ to obtain intermediate 2-chloro-2-hydroxypropyl cellulose ether (CHPC).