功能高分子膜的合成及其对海水中铀的吸脱附过程的研究
发布时间：2018-08-26 18:17
【摘要】：为了提高从海水中提取铀的效率,实验室制备了具有功能膜的螯合电极。以镍片为基材,顺次组装上KH550、用二茂铁衍生物改性的聚氨酯(PU)预聚物、丙烯腈与丙烯酸的共聚物P(AN-co-AA),制备薄膜电极,然后再将薄膜电极直接浸入盐酸羟胺溶液中,制得带有偕胺肟基团的功能电极。用FT-IR和1H NMR表征各步的合成产物,用SEM表征电极的表面形貌,用循环伏安法表征电极的电化学行为,用荧光光度法测定铀的含量。(1)用自组装的方法制备所需的薄膜电极。用电导率法,确定KH550溶液的最佳配比为Vkh550:V乙醇：V水= 1:74:25,在最佳配比下进行水解,得到最佳的水解时间是30min。通过对比电极组装前后的质量和SEM表征,得出结论：电极在KH550溶液、0.3%PU预聚物/乙酸乙酯溶液中的最佳组装时间分别为2min、 10min,丙烯酸与丙烯腈的单体质量比为1：9时,电极在质量分数为0.45%的P(AA-co-AN)/DMF溶液中的最佳组装时间为7min,制得薄膜电极。(2)薄膜电极在0.01mol/L的盐酸羟胺溶液中进行偕胺肟化反应,通过SEM表征,得到最佳偕胺肟化时间为50mmin,制得功能电极。(3)吸附速率随着吸附的时间、动静态条件的变化而发生改变,静态吸附平衡时间为8天,平衡吸附量为6.3mg/g吸附剂。(4)通过SEM表征,观察到功能电极的表面形貌在吸附前后有较大的改变,吸附效果良好。(5)在海水中吸附铀后的电极可选择3%的NaCl溶液或pH=6.8磷酸盐缓冲液作为支持电解质,脱附电压分别为0.25V、0.72V。
[Abstract]:In order to improve the efficiency of uranium extraction from seawater, a chelating electrode with functional membrane was prepared. Polyurethane (PU) prepolymer modified by ferrocene derivative of KH550, and copolymer P (AN-co-AA) of acrylonitrile and acrylic acid were prepared with nickel sheet as substrate, and then directly immersed in hydroxylamine hydrochloride solution. Functional electrode with amidoxime group was prepared. The synthesized products were characterized by FT-IR and 1H NMR, the surface morphology of the electrode was characterized by SEM, the electrochemical behavior of the electrode was characterized by cyclic voltammetry, and the content of uranium was determined by fluorescence spectrophotometry. (1) the thin film electrode was prepared by self-assembly method. By using the conductivity method, the optimum ratio of KH550 solution was determined as Vkh550:V ethanol: v water = 1: 74: 25. The optimum hydrolysis time was 30 min. By comparing the mass and SEM characterization before and after the electrode assembly, it is concluded that the optimum assembling time of the electrode in the prepolymer / ethyl acetate solution of KH550 solution is 2 min and 10 min, respectively, and the mass ratio of acrylic acid to acrylonitrile is 1:9. The best assembly time of the electrode in P (AA-co-AN) / DMF solution with 0.45% mass fraction was 7 min. (2) Oximation reaction of the thin film electrode in hydroxylamine hydrochloride solution of 0.01mol/L was carried out and characterized by SEM. The optimum amidoximation time was 50 min, and the functional electrode was prepared. (3) the adsorption rate changed with the adsorption time and the dynamic and static conditions. The static adsorption equilibrium time was 8 days, and the equilibrium adsorption amount was 6.3mg/g adsorbent. (4) the adsorption rate was characterized by SEM. It was observed that the surface morphology of the functional electrode changed greatly before and after adsorption, and the adsorption effect was good. (5) after adsorption of uranium in seawater, 3% NaCl solution or pH=6.8 phosphate buffer solution could be selected as the supporting electrolyte, and the desorption voltage was 0.25 V / 0.72 V, respectively.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.2;O647.3
本文编号：2205755
[Abstract]:In order to improve the efficiency of uranium extraction from seawater, a chelating electrode with functional membrane was prepared. Polyurethane (PU) prepolymer modified by ferrocene derivative of KH550, and copolymer P (AN-co-AA) of acrylonitrile and acrylic acid were prepared with nickel sheet as substrate, and then directly immersed in hydroxylamine hydrochloride solution. Functional electrode with amidoxime group was prepared. The synthesized products were characterized by FT-IR and 1H NMR, the surface morphology of the electrode was characterized by SEM, the electrochemical behavior of the electrode was characterized by cyclic voltammetry, and the content of uranium was determined by fluorescence spectrophotometry. (1) the thin film electrode was prepared by self-assembly method. By using the conductivity method, the optimum ratio of KH550 solution was determined as Vkh550:V ethanol: v water = 1: 74: 25. The optimum hydrolysis time was 30 min. By comparing the mass and SEM characterization before and after the electrode assembly, it is concluded that the optimum assembling time of the electrode in the prepolymer / ethyl acetate solution of KH550 solution is 2 min and 10 min, respectively, and the mass ratio of acrylic acid to acrylonitrile is 1:9. The best assembly time of the electrode in P (AA-co-AN) / DMF solution with 0.45% mass fraction was 7 min. (2) Oximation reaction of the thin film electrode in hydroxylamine hydrochloride solution of 0.01mol/L was carried out and characterized by SEM. The optimum amidoximation time was 50 min, and the functional electrode was prepared. (3) the adsorption rate changed with the adsorption time and the dynamic and static conditions. The static adsorption equilibrium time was 8 days, and the equilibrium adsorption amount was 6.3mg/g adsorbent. (4) the adsorption rate was characterized by SEM. It was observed that the surface morphology of the functional electrode changed greatly before and after adsorption, and the adsorption effect was good. (5) after adsorption of uranium in seawater, 3% NaCl solution or pH=6.8 phosphate buffer solution could be selected as the supporting electrolyte, and the desorption voltage was 0.25 V / 0.72 V, respectively.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.2;O647.3
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