鋼鐵鹽酸酸洗廢液資源化利用:電解法制備納米氧化鐵的研究
發(fā)布時間:2018-03-14 17:07
本文選題:鋼鐵鹽酸酸洗廢液 切入點:資源化 出處:《浙江大學》2017年碩士論文 論文類型:學位論文
【摘要】:鹽酸作為鋼鐵酸洗工序常用的酸洗清潔劑被鋼鐵生產(chǎn)企業(yè)大量使用。我國每年產(chǎn)生大量的鋼鐵鹽酸酸洗廢液,國內(nèi)已將其列入危險廢物名錄。目前常規(guī)的處置方式以石灰乳中和、蒸餾回收鹽酸、鐵系混凝劑制備等方法為主,但從資源利用的角度來講卻是經(jīng)濟性欠佳。本文以鋼鐵鹽酸酸洗廢液為研究對象,設計了專門的電解試驗裝置,探究以電解法處理鋼鐵鹽酸酸洗廢液,以廢液中的鐵離子為原材料,制備高附加值納米氧化鐵,從而提高鋼鐵鹽酸酸洗廢液的資源化利用效率。本文設計了一個由陽離子交換膜分隔成兩室的電解試驗裝置,以釕鉑鈦合金作為陰陽電極,陽極室添加過濾之后的低酸度鋼鐵鹽酸酸洗廢液,陰極室添加一定濃度的NaCl溶液和分散劑,以外部直流穩(wěn)壓電源提供電流,進行電解法制備納米氧化鐵試驗。采用單因素試驗法探究了分散劑種類、電流密度、反應溫度、煅燒溫度等試驗條件對納米氧化鐵制備的影響,以TEM圖像表征的方式,通過對比粒徑、形貌、分散性指標,優(yōu)化試驗條件。再以分散劑用量、電流密度、反應溫度、煅燒溫度為指標,進行四因素三水平的L9(34)正交試驗,并以納米氧化鐵產(chǎn)品質量(g)、Fe2O3含量(%)、電流效率(%)以及粒徑(nm)為指標,探究納米氧化鐵制備的最佳試驗條件,最后以最佳試驗條件制備納米氧化鐵并進行相應表征。通過單因素電解試驗,電流密度確定在80A/m2上下;相對而言,單獨添加聚乙二醇的分散效果更優(yōu);反應溫度初步確定為20~30℃;煅燒溫度大約為600℃。正交試驗結果顯示,產(chǎn)品質量、Fe2O3含量、電流效率和粒徑的顯著性影響因素分別為電流密度、反應溫度、分散劑用量與煅燒溫度。通過正交試驗結果與直觀分析數(shù)據(jù)的分析,確定最佳試驗條件為分散劑采用聚乙二醇,添加量為1.0g,電流密度100A/m2,反應溫度30℃,煅燒溫度600℃。最佳試驗條件下制備得到橢圓短棒狀納米氧化鐵微粒,經(jīng)XRD分析確定晶型為α-Fe2O3。平均粒徑為68nm,Fe2O3含量可達99.53%,此兩項指標可達到《工業(yè)氧化鐵(HG/T2574-2009)》合格品以上的要求,且Fe2O3含量單項指標還可以滿足《氧化鐵顏料(GB/T1863-2008)》氧化鐵顏料紅A類的要求;電流效率達到了 91.80%,Fe回收率為34.89%。
[Abstract]:Hydrochloric acid is widely used in iron and steel enterprises as the common acid cleaning agent in iron and steel pickling process. A large amount of acid pickling liquid of iron and steel is produced every year in China. It has been listed in the list of hazardous wastes in China. At present, the usual methods of disposal are lime milk neutralization, distillation and recovery of hydrochloric acid, preparation of ferric coagulant, etc. However, from the point of view of resource utilization, it is not economical enough. In this paper, a special electrolytic test device is designed to deal with the acid pickling waste of iron and steel hydrochloric acid by electrolytic method, taking the acid pickling liquid of iron and steel hydrochloric acid as the research object. Using iron ion in waste liquid as raw material, high value-added nanometer ferric oxide was prepared to improve the utilization efficiency of iron and steel hydrochloric acid acid pickling waste liquid. An electrolytic test device separated by cation exchange membrane into two chambers was designed in this paper. Ruthenium platinum-titanium alloy was used as the cathode electrode, the anodic chamber was filled with filtered low-acidity acid acid pickling liquid of iron and steel, and the cathode chamber was filled with certain concentration of NaCl solution and dispersant. The current was provided by external DC power supply. The effects of the kinds of dispersant, current density, reaction temperature and calcination temperature on the preparation of nanometer iron oxide were investigated by single factor method. By comparing particle size, morphology, dispersity index, optimizing test conditions, and taking dispersant dosage, current density, reaction temperature and calcination temperature as indexes, the orthogonal test was carried out at four factors and three levels. Taking the content of Fe _ 2O _ 3, current efficiency and particle size of nanometer iron oxide as the index, the optimum experimental conditions for the preparation of nanometer iron oxide were studied, and the content of Fe _ 2O _ 3 and the content of Fe _ 2O _ 3 in nanometer iron oxide were studied. Finally, the nanometer ferric oxide was prepared under the optimum experimental conditions and characterized accordingly. The current density was about 80 A / m ~ 2 by single factor electrolysis test, and the dispersion effect of adding polyethylene glycol alone was better. The reaction temperature is 20 ~ 30 鈩,
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