过硫酸铵对微晶石墨混酸提纯的强化作用

Strengthening effect of ammonium persulfate on the mixed-acid purification of microcrystalline graphite

  • 摘要: 微晶石墨主要的杂质矿物包括石英、云母、绿泥石和硫化矿等。现有的酸浸纯化工艺存在杂质矿物难溶和杂质二次沉淀等问题。本文以盐酸和氢氟酸为主要浸出剂,通过添加过硫酸铵的方式,改变浸出体系的氧化性,强化微晶石墨酸浸纯化的效果。酸浸实验表明,加入过硫酸铵后,微晶石墨的酸浸纯化效果得到明显改善,石墨的固定碳含量由原来的98.0%提高至98.4%。由热力学分析可知,常温体系下的黄铁矿不能与氢氟酸和盐酸自发反应,而硫酸铵的加入能够促进黄铁矿与氢氟酸和盐酸的反应。此外,杂质云母和绿泥石在和氢氟酸反应的过程中易产生六氟硅酸钾沉淀,而混合酸中的盐酸能够在一定程度上抑制六氟硅酸钾沉淀的生成,提高纯化的效率。通过对酸浸后石墨的表面结构和晶体结构分析可知,氧化剂过硫酸铵的加入并不会影响石墨的表面结构和晶体结构。

     

    Abstract: The primary impurity minerals in microcrystalline graphite include quartz, mica, chlorite, and sulfide minerals (such as pyrite). Current acid leaching purification processes face challenges, including the low solubility of impurities and the occurrence of secondary precipitation. In this study, hydrochloric acid (HCl) and hydrofluoric acid (HF) were used as the primary leaching agents, and ammonium persulfate ((NH4)2S2O8) was introduced to enhance the oxidative properties of the leaching system, thereby strengthening the purification effect. Acid leaching experiments demonstrated that the fixed carbon content of graphite increased from 98.0% to 98.4% with the addition of ammonium persulfate, indicating a significant improvement in the purification efficiency. Thermodynamic analysis revealed that while pyrite cannot spontaneously react with HF and HCl at ambient temperature, the addition of ammonium persulfate promoted its dissolution. Furthermore, it was found that the reaction of mica and chlorite with HF tended to generate potassium hexafluorosilicate (K2SiF6) precipitates. However, the presence of hydrochloric acid in the mixed acid system effectively suppressed the formation of these precipitates to a certain extent, thereby enhancing the purification efficiency. Structural characterization of the purified graphite indicated that the introduction of ammonium persulfate did not adversely affect the surface morphology or the crystalline structure of the microcrystalline graphite.

     

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