离子交换法除去合成羟胺反应液中的铁、铬离子

【作者】 张晓东；

【导师】 黄可龙；

【作者基本信息】 中南大学 ， 应用化学， 2002， 硕士

【摘要】 本文研究了羟胺生产过程中催化剂失活和溶液排放的原因，采用离子交换法除去溶液中的铁（Ⅱ）、铬（Ⅲ）等离子。通过吸附剂和解吸剂的筛选，吸附条件和解吸条件的考察，确定了SL-406酸性螯合树脂在流速1／10（V／V／min）条件下吸附；应用1％EDTA+1mol／LHCl的混合溶液在流速1／10（V／V／min）条件下可同时解吸铁和铬离子；树脂的饱和吸附容量可达1.8mmol／g，铁（Ⅱ）净化率达100％，铬（Ⅲ）净化率为70％。 本文还研究了溶液中铁、铬离子的分光光度法，利用邻二氮菲与铁（Ⅱ）生成红色化合物来测定铁离子，最大吸收峰在510nm，摩尔吸光系数=1.12×10³L·mol^-1·cm^-1，铁（Ⅱ）在0～0.1mg／50ml范围内符合比尔定律，该法的相对误差小于5％，回收率在98％和103％之间。利用铬（Ⅲ）与H₃PO₄生成绿色配合物的显色反应测定磷酸体系中的铬（Ⅲ）离子，最大吸收峰在660nm，摩尔吸光系数=1.4×10²L·mol^-1·cm^-1，铬（Ⅲ）在0～0.5mg／25ml范围内符合比尔定律，该法的相对误差小于5％，回收率在98％和103％之间。 本文的研究成果为工业中除去合成羟胺反应液中的铁、铬离子提供了重要的实验依据。更多还原

【Abstract】 The factors of the catalyst poising and the solutions being discharged have been studied in this article, which were caused by iron(Ⅱ), chromium(Ⅲ) ion in the solutions. The ion exchanging method to remove the iron(Ⅱ), chromiuni(Ⅲ) ion from the solutions has been applied in the process of synthesize hydroxylamine, and various adsorbents, the influence of different adsorption conditions, eluents , the desorption conditions have been investigated. Finally, we choosed the SL-406 chelation resin as the best adsorbent. The results showed that the best condition for adsorption was flow rate 1/10(v/v/min), and that the best condition for desorption iron( Ⅱ), chromium(Ⅲ) at the same time was flow rate l/10(v/v/min) by the l%EDTA+lmol/L HC1 solutions. The adsorption capacity of SL-406 resin was up to 1.8mmol/g. Elimination percent of iron( Ⅱ) ion was approximately 100%, and that of chromium(Ⅲ) ion was 70%.Spectrophotometries of iron(Ⅱ), chromium(Ⅲ) ion were also studied. Iron(Ⅱ) ion was determined by reacting with O-phenanthroline to form a colour complex (A max=510nm), which obeyed Beer’s law in the range of 0~0.1mg/50ml. Its molar adsorption coefficient was 1.12 × 103 L ·mor-1·m-1 , its relative accuracy was 5%, and its recovery percent was between 98% and 103%. Chromium(III) ion was determined by reacting with H3PO4 to form a colour complex (A. max=660nm), which obeyed Beer’s law in the range of 0~0.5mg/25ml. Its molar adsorption coefficient was 1.4 ×10 L·mol-1·cm4 , its relative accuracy was 5%, and its recovery percent was between 98% and 103%.The conclusion of the article has provided the important reference for removal of iron(Ⅱ), chromium( Ⅲ) ion from the reacting solutions of the synthesize of hydroxylamine in industry.更多还原