【摘要】：本文的目的是找到一條經(jīng)濟(jì)、綠色、高效的方法合成六水合高氯酸鎳,以期實(shí)現(xiàn)工業(yè)化進(jìn)程。選擇廢舊的鎳氫電池作為研究對(duì)象,采取破碎分離、酸浸、萃取和反萃取等手段從中提取硫酸鎳,進(jìn)而沉淀轉(zhuǎn)化為堿式碳酸鎳,并以此作為鎳源合成高氯酸鎳晶體。最終實(shí)現(xiàn)六水合高氯酸鎳的經(jīng)濟(jì)、綠色、高效的工業(yè)化生產(chǎn)。針對(duì)廢舊鎳氫電池進(jìn)行酸浸實(shí)驗(yàn)。選擇廢舊電池的負(fù)極材料,采取機(jī)械分離的手段得到負(fù)極的儲(chǔ)氫材料,然后選用H2SO4酸浸。實(shí)驗(yàn)條件為:3mol/L的H2SO4溶液,固液比為1:5,浸出時(shí)間為4h,浸出溫度為95℃。得到結(jié)果為稀土金屬的沉淀率達(dá)到95%,而Ni與Co等元素浸出率高達(dá)99.5%,可以達(dá)到初步分離的效果。隨后進(jìn)行正負(fù)極活性金屬粉末的整體浸出實(shí)驗(yàn),得到最佳的浸出條件是:3mol/L的硫酸溶液,液固比為7.5:1,浸出溫度為95℃,浸出時(shí)間為4h。在該條件下,可以實(shí)現(xiàn)稀土金屬與其他金屬的初步分離。用5mol/L的NaOH溶液調(diào)節(jié)浸出液的pH值,浸出液中的稀土金屬以各自硫酸鹽的形式從浸出液中沉淀析出,稀土金屬的沉淀析出率可以達(dá)到98%,pH值控制在0.6～1.2之間。通過(guò)浸出和調(diào)節(jié)pH值,將廢舊鎳氫電池中99%以上的稀土金屬以稀土金屬硫酸鹽沉淀的形式回收并加以利用,不需要再進(jìn)行加熱萃取等步驟。選用湖南宏邦提供的HBL110萃取劑,在萃原液中該萃取劑的萃取先后順序?yàn)?NiCoZn。結(jié)論是:萃取劑濃度為50%,空載有機(jī)相萃取劑pH為3,萃原液pH為2,相比為7,萃取級(jí)數(shù)為5,大部分的鎳進(jìn)入有機(jī)相,其他干擾金屬元素全都留在萃余液中。隨后用硫酸進(jìn)行鎳離子的反萃,最佳反萃條件:室溫、反萃時(shí)間為7min、硫酸濃度為100g/L、有機(jī)相和水相的比值為5、一級(jí)反萃,反萃率可以達(dá)到99.6%。硫酸鎳合成堿式碳酸鎳最佳條件:0.5mol/L硫酸鎳溶液,滴入到盛有飽和碳酸鈉的反應(yīng)器中(反加法),控制終點(diǎn)pH值為8.5,反應(yīng)溫度為70℃,沉淀過(guò)濾、去離子水沖洗去雜質(zhì)離子、干燥、得到堿式碳酸鎳粉末。通過(guò)堿式碳酸鎳和30%的高氯酸反應(yīng),得到純度較高的六水合高氯酸鎳。
[Abstract]:The purpose of this paper is to find an economical, green and efficient method for the synthesis of nickel perchlorate hexahydrate. The waste Ni-MH battery was selected as the research object. Nickel sulfate was extracted by crushing separation, acid leaching, extraction and back-extraction, and then precipitated into basic nickel carbonate, which was used as a nickel source to synthesize nickel perchlorate crystals. The final realization of nickel perchlorate hexahydrate economy, green, efficient industrial production. Acid leaching experiments were carried out for waste Ni-MH batteries. The negative electrode material of waste battery is selected, the hydrogen storage material of negative electrode is obtained by mechanical separation, and then H2SO4 acid leaching is selected. The experimental conditions are as follows: the H2SO4 solution of 3mol/L, the ratio of solid to liquid is 1: 5, the leaching time is 4 h, and the leaching temperature is 95 鈩，

本文編號(hào)：2270298