【摘要】：針對(duì)冶煉系統(tǒng)產(chǎn)出的各種含銻廢棄料得不到有效回收利用,同時(shí)對(duì)環(huán)境造成污染的現(xiàn)狀,在對(duì)銅陽(yáng)極泥分銻渣物性分析的基礎(chǔ)上,提出“硫化鈉堿浸—氧化沉銻—精制除雜”銻酸鈉生產(chǎn)新工藝,為銻資源的回收再利用開(kāi)辟了新的途徑和實(shí)際生產(chǎn)工藝提供有意義的參考。本課題針對(duì)銻渣硫化鈉堿浸和空氣催化氧化硫代亞銻酸鈉制備銻酸鈉過(guò)程及其動(dòng)力學(xué)進(jìn)行研究,得出以下結(jié)論:(1)對(duì)銻渣采用Na2S+Na OH堿性浸出試驗(yàn),考察了多種因素對(duì)浸銻過(guò)程的影響,確定了浸出最佳條件為:硫化鈉濃度165 g·L-1,氫氧化鈉濃度30-40 g·L-1,固液比1:5,浸出溫度85℃-90℃,反應(yīng)時(shí)間1h-1.5h。按上述條件試驗(yàn),銻浸出率95%,浸出渣含銻6%。Pb、Cu、Ag、Fe等金屬入渣率97%,實(shí)現(xiàn)了銻與其他金屬的分離及雜質(zhì)金屬元素有效的富集。(2)對(duì)銻渣的堿浸過(guò)程動(dòng)力學(xué)研究發(fā)現(xiàn),在55℃-85℃溫度范圍內(nèi),浸出過(guò)程屬于化學(xué)反應(yīng)控制,溫度對(duì)浸出率有顯著影響,反應(yīng)表觀活化能為47.86 k J·mol-1。(3)通過(guò)對(duì)浸出液采用空氣催化氧化制備粗銻酸鈉實(shí)驗(yàn)研究,確定了最佳銻氧化條件為:高錳酸鉀加入量0.75 g·L-1,鄰苯二酚加入量不超過(guò)0.5 g·L-1,鼓風(fēng)強(qiáng)度1.415m3·m-2·min-1,氫氧化鈉過(guò)量系數(shù)1.5-1.6,反應(yīng)溫度75℃-85℃,氧化時(shí)間6 h-8 h。銻的氧化率達(dá)到98.06%以上,沉銻后液中銻濃度低于0.3 g·L-1。(4)在氧化硫代亞銻酸鈉動(dòng)力學(xué)研究過(guò)程中,聯(lián)合運(yùn)用孤立法及半衰期法處理實(shí)驗(yàn)結(jié)果,求出該反應(yīng)動(dòng)力學(xué)方程式及其表觀活化能。在催化條件下該反應(yīng)動(dòng)力學(xué)方程式:1.1610.4889Sb]×k=[Na OH][ ×dtd[Sb]-反應(yīng)表觀活化能為5.04 k J·mol-1,確定氧化反應(yīng)控制步驟是擴(kuò)散傳質(zhì)控制。(5)粗銻酸鈉通過(guò)酸溶除雜精制,獲得具有雜質(zhì)含量低、白度高優(yōu)質(zhì)銻酸鈉產(chǎn)品。SEM分析表明,銻酸鈉顆粒分布均勻,分散性好,顆粒尺寸大,平均粒度達(dá)到80μm。銻總回收率為91.23%。
[Abstract]:In view of the fact that various antimony waste materials produced by smelting system can not be effectively recycled and polluted to the environment, based on the analysis of the properties of antimony separation slag from copper anode slime, A new process for the production of sodium antimony by alkali leaching, oxidation precipitation, purification and removal of impurities by sodium sulfide is proposed, which provides a valuable reference for the recovery and reuse of antimony resources. The preparation and kinetics of sodium antimonate from antimony residue by alkaline leaching of sodium sulphide and air catalyzed oxidation of sodium antimonite were studied in this paper. The following conclusions were obtained: (1) the alkaline leaching experiment of antimony residue with Na2S NaOH was carried out. The effects of various factors on antimony leaching were investigated. The optimum leaching conditions were determined as follows: concentration of sodium sulfide 165 g L -1, concentration of sodium hydroxide 30-40 g L -1, ratio of solid to liquid 1: 5, leaching temperature 85 鈩，

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