【摘要】：為了提高從海水中提取鈾的效率,實驗室制備了具有功能膜的螯合電極。以鎳片為基材,順次組裝上KH550、用二茂鐵衍生物改性的聚氨酯(PU)預聚物、丙烯腈與丙烯酸的共聚物P(AN-co-AA),制備薄膜電極,然后再將薄膜電極直接浸入鹽酸羥胺溶液中,制得帶有偕胺肟基團的功能電極。用FT-IR和1H NMR表征各步的合成產物,用SEM表征電極的表面形貌,用循環(huán)伏安法表征電極的電化學行為,用熒光光度法測定鈾的含量。(1)用自組裝的方法制備所需的薄膜電極。用電導率法,確定KH550溶液的最佳配比為Vkh550:V乙醇：V水= 1:74:25,在最佳配比下進行水解,得到最佳的水解時間是30min。通過對比電極組裝前后的質量和SEM表征,得出結論：電極在KH550溶液、0.3%PU預聚物/乙酸乙酯溶液中的最佳組裝時間分別為2min、 10min,丙烯酸與丙烯腈的單體質量比為1：9時,電極在質量分數(shù)為0.45%的P(AA-co-AN)/DMF溶液中的最佳組裝時間為7min,制得薄膜電極。(2)薄膜電極在0.01mol/L的鹽酸羥胺溶液中進行偕胺肟化反應,通過SEM表征,得到最佳偕胺肟化時間為50mmin,制得功能電極。(3)吸附速率隨著吸附的時間、動靜態(tài)條件的變化而發(fā)生改變,靜態(tài)吸附平衡時間為8天,平衡吸附量為6.3mg/g吸附劑。(4)通過SEM表征,觀察到功能電極的表面形貌在吸附前后有較大的改變,吸附效果良好。(5)在海水中吸附鈾后的電極可選擇3%的NaCl溶液或pH=6.8磷酸鹽緩沖液作為支持電解質,脫附電壓分別為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.
【學位授予單位】：青島科技大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TB383.2;O647.3

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