離子液體的制備及萃取電鍍污泥中金屬的研究
發(fā)布時(shí)間:2019-03-17 19:22
【摘要】:電鍍行業(yè)作為基礎(chǔ)產(chǎn)業(yè)之一,為我國經(jīng)濟(jì)快速發(fā)展做出了巨大貢獻(xiàn)。但與此同時(shí),電鍍行業(yè)會(huì)產(chǎn)生大量的電鍍污泥,其中含有大量有毒有害的金屬,若得不到有效的處理,將會(huì)對(duì)環(huán)境造成巨大的影響。離子液體作為新型綠色溶劑,廣泛應(yīng)用于各個(gè)行業(yè)中,本文主要利用離子液體的萃取金屬特性,將其應(yīng)用于回收電鍍污泥中金屬,使電鍍污泥達(dá)到變廢為寶的目的。1、本文主要采用微波輔助兩步法合成1-丁基-3-甲基咪唑六氟磷酸鹽([BMIM][PF_6])、1-己基-3-甲基咪唑六氟磷酸鹽([HMIM][PF_6])、1-辛基-3-甲基咪唑六氟磷酸鹽([OMIM][PF_6])3種咪唑類離子液體,并對(duì)其粘度進(jìn)行測(cè)定。利用合成的3種離子液體對(duì)Pb~(2+)、Zn~(2+)、Ni~(2+)、Cd~(2+)、Co~(2+)5種金屬離子進(jìn)行萃取實(shí)驗(yàn),結(jié)果表明[BMIM][PF_6]對(duì)5種金屬的萃取量最大。利用FT-IR、1HNMR、HPLC表征手段對(duì)[BMIM][PF_6]的結(jié)構(gòu)和含量進(jìn)行了測(cè)定。2、采用[BMIM][PF_6]、[BMIM][PF_6]-雙硫腙兩種體系分別對(duì)Pb~(2+)、Zn~(2+)、Ni~(2+)、Cd~(2+)、Co~(2+)5種金屬離子的萃取性能進(jìn)行了研究。在最佳萃取體系[BMIM][PF_6]-雙硫腙條件下,研究了溫度、時(shí)間、p H、金屬離子初始濃度等因素對(duì)萃取性能的影響,并對(duì)Pb~(2+)、Zn~(2+)、Ni~(2+)3種金屬離子做了正交實(shí)驗(yàn),得到最佳萃取條件。3、以實(shí)際電鍍污泥為原料,優(yōu)化酸浸出時(shí)的工藝條件,探究固液比、時(shí)間、溫度對(duì)金屬浸出的影響,最終得到最佳工藝條件為:固液比為1:10,攪拌時(shí)間為100min,溫度40℃。4、以硫酸浸出液為原料,采用分步沉淀法和溶劑萃取法對(duì)溶液中金屬進(jìn)行分離。銅的萃取劑和反萃劑分別為LIX984N和硫酸,萃取的最佳條件為:萃取劑和金屬溶液體積之比為1:3,p H=1.5,攪拌時(shí)間為3min,萃取溫度為45℃,萃取率可達(dá)96.7%;反萃硫酸最佳濃度為5mol/L,反萃率可達(dá)84.2%。鋅的萃取劑和反萃劑分為為[BMIM][PF_6]-雙硫腙和硫酸,鋅采用4級(jí)萃取,萃取率可達(dá)95.5%;反萃使用3mol/L的硫酸,反萃級(jí)數(shù)為3級(jí),反萃率為81.7%。在最優(yōu)的工藝條件下,對(duì)電鍍污泥進(jìn)行放大處理,經(jīng)酸浸、分步沉淀、萃取等步驟之后,分別得到硫酸銅、硫酸鎳、硫酸鋅。Cu回收率為77.37%,Ni回收率為78%,Zn回收率為73.9%。
[Abstract]:As one of the basic industries, electroplating industry has made great contribution to the rapid development of China's economy. But at the same time, electroplating industry will produce a large number of electroplating sludge, which contains a large number of toxic and harmful metals, if not treated effectively, it will have a great impact on the environment. Ionic liquids, as a new green solvent, are widely used in various industries. In this paper, the metal extraction properties of ionic liquids are mainly used to recover metal from electroplating sludge, and the electroplating sludge is used to turn waste into treasure. In this paper, 1-Ding Ji-3-methylimidazole hexafluorophosphate ([BMIM] [PF_6]) and 1-hexyl-3-methylimidazole hexafluorophosphate ([HMIM] [PF_6]) were synthesized by microwave assisted two-step method. Three kinds of imidazole ionic liquids, 1-octyl-3-methylimidazole hexafluorophosphate ([OMIM] [PF_6]), and their viscosity were determined. Five metal ions (Pb~ (2), Zn~ (2), Ni~ (2), Cd~ (2), Co~ (2) were extracted with three synthetic ionic liquids. The results showed that [BMIM] [PF_6] had the highest extraction amount of five metals. The structure and content of [BMIM] [PF_6] were determined by FT-IR,1HNMR,HPLC. 2. Pb~ (2) and Zn~ (2) were determined by [BMIM] [PF_6], [BMIM] [PF_6]-dithizone, respectively. The extraction properties of Ni~ (2), Cd~ (2) and Co~ (2) were studied. Under the optimum extraction system [BMIM] [PF_6]-dithizone, the effects of temperature and time, p H, initial concentration of metal ions on the extraction performance were studied, and Pb~ (2), Zn~ (2), etc. The orthogonal experiment of Ni~ (2) three kinds of metal ions was carried out, and the optimum extraction conditions were obtained. 3. The effect of solid-liquid ratio, time and temperature on the leaching of metal was studied by optimizing the technological conditions of acid leaching with the actual electroplating sludge as the raw material, and the effects of solid-liquid ratio, time and temperature on the leaching of metal were studied. The optimum technological conditions are as follows: the ratio of solid to liquid is 10, stirring time is 100min, temperature is 40 鈩,
本文編號(hào):2442621
[Abstract]:As one of the basic industries, electroplating industry has made great contribution to the rapid development of China's economy. But at the same time, electroplating industry will produce a large number of electroplating sludge, which contains a large number of toxic and harmful metals, if not treated effectively, it will have a great impact on the environment. Ionic liquids, as a new green solvent, are widely used in various industries. In this paper, the metal extraction properties of ionic liquids are mainly used to recover metal from electroplating sludge, and the electroplating sludge is used to turn waste into treasure. In this paper, 1-Ding Ji-3-methylimidazole hexafluorophosphate ([BMIM] [PF_6]) and 1-hexyl-3-methylimidazole hexafluorophosphate ([HMIM] [PF_6]) were synthesized by microwave assisted two-step method. Three kinds of imidazole ionic liquids, 1-octyl-3-methylimidazole hexafluorophosphate ([OMIM] [PF_6]), and their viscosity were determined. Five metal ions (Pb~ (2), Zn~ (2), Ni~ (2), Cd~ (2), Co~ (2) were extracted with three synthetic ionic liquids. The results showed that [BMIM] [PF_6] had the highest extraction amount of five metals. The structure and content of [BMIM] [PF_6] were determined by FT-IR,1HNMR,HPLC. 2. Pb~ (2) and Zn~ (2) were determined by [BMIM] [PF_6], [BMIM] [PF_6]-dithizone, respectively. The extraction properties of Ni~ (2), Cd~ (2) and Co~ (2) were studied. Under the optimum extraction system [BMIM] [PF_6]-dithizone, the effects of temperature and time, p H, initial concentration of metal ions on the extraction performance were studied, and Pb~ (2), Zn~ (2), etc. The orthogonal experiment of Ni~ (2) three kinds of metal ions was carried out, and the optimum extraction conditions were obtained. 3. The effect of solid-liquid ratio, time and temperature on the leaching of metal was studied by optimizing the technological conditions of acid leaching with the actual electroplating sludge as the raw material, and the effects of solid-liquid ratio, time and temperature on the leaching of metal were studied. The optimum technological conditions are as follows: the ratio of solid to liquid is 10, stirring time is 100min, temperature is 40 鈩,
本文編號(hào):2442621
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