污泥源腐殖酸的提取及沉淀低浓度稀土作用机制

Extraction of humic acid derived from sludge and mechanism of low concentration rare earth precipitation

  • 摘要: 采用焦磷酸钠法和碱溶酸析法分别从剩余污泥中提取污泥源腐殖酸。利用扫描电镜、红外光谱和三维荧光光谱对2种腐殖酸进行表征分析,并对比了二者对低浓度稀土离子的沉淀效果。结果表明:2种腐殖酸中均含有大量的羧酸类、胺类、羟基类官能团,但焦磷酸钠法提取的S-HA-1中官能团的种类更多、含量更高;当沉淀稀土离子浓度为103.40 mg/L时,2种腐殖酸对稀土的沉淀率分别达97.30%和91.18%,沉淀物中稀土元素重量百分比总和分别为31.73%和28.64%,S-HA-1沉淀效果较优。采用S-HA-1为沉淀剂,稀土离子浓度为51.70 mg/L时,通过单因素实验与响应面优化实验确定了较优反应条件:腐殖酸浓度0.25 g/L,反应时间56.53 min,搅拌速率106.27 r/min,反应温度40 ℃,pH=5.90,在此条件下,稀土沉淀率≥ 98%。利用能谱和红外光谱分析稀土沉淀物发现,沉淀过程中稀土离子与S-HA表面的酚羟基和羧基等官能团发生了一系列物理化学反应,形成腐殖酸-稀土絮状体沉淀。研究结果表明,从剩余污泥提取腐殖酸低浓度稀土离子沉淀剂,既能实现沉淀剂再利用,又能回收稀土资源。

     

    Abstract: Extracted from surplus sludge by the sodium pyrophosphate and alkaline solution-acid extraction methods, respectively, sludge-derived humic acids were characterized by scanning electron microscopy, infrared spectroscopy and three-dimensional fluorescence. The precipitation effect of the two humic acids on the low concentration of rare earth ions was also compared. The results show that both humic acids contain a large amount of carboxylic acids, amines and hydroxyl groups, but the types and contents of functional groups are higher in S-HA-1 extracted by the sodium pyrophosphate method. When the rare earth ion concentration is 103.40 mg/L, the precipitation rates of rare earth elements are 97.30% and 91.18%, and the total weight percentages of rare earth elements in the sediment are 31.73% and 28.64%, respectively, with the best precipitation effec of S-HA-1. With S-HA-1 as a precipitatant, determined by a single-factor experiment and response surface optimization experiment, the optimal reaction conditions are the rare earth ion concentration of 51.70 mg/L, humic acid concentration of 0.25 g/L, the reaction time of 56.53 min, the stirring rate of 106.27 r/min, the reaction temperature at 40 ℃, pH of 5.90, and the rare earth precipitation rate ≥ 98%. The analysis of rare earth precipitates by energy spectrum and infrared spectrum revealed that a series of physical and chemical reactions occured between rare earth ions and functional groups such as phenolic hydroxyl groups and carboxyl groups on the surface of S-HA during precipitation, forming humic acid-rare earth flocculent precipitates. The results show that humic acids can be extracted from residual sludge to be the low-concentration rare earth ion precipitatants, which can not only achieve precipitant reuse, but also recover rare earth resources.

     

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