Experiment Study on Preparation of Graphene by Extracting Graphite from Graphite Tailings in Luobei
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摘要:
石墨烯独特的结构特性与优异的理化性质，使其具有广阔的应用前景。以萝北某石墨尾矿为对象，采用粉碎、超声剥离、重力沉降，提取石墨尾矿中石墨微纳米片，然后进行提纯剥离制备石墨烯。结果表明，研磨获得d50为2.5 µm左右的尾矿颗粒，超声剥离处理6 min，重力沉降进行石墨富集，获得石墨微片碳含量最高达9.72%，石墨回收率达80.01%，石墨微片经提纯后得到固定碳含量为98.1%、层数约为20层左右的石墨微纳米片。采用高压微射流均质机进行剥离制备多层石墨烯，石墨微片、水及分散剂配比为0.2 mg∶1 mL∶0.001 mg，高压微射流均质机的压力80 MPa，进行高压分散循环25次后，剥离得到的石墨烯片厚度在10层以下、片径在3 μm以上，制成具有较高晶体质量的石墨烯。石墨尾矿制备石墨烯既有利于拓展石墨烯原料范围又有利于实现石墨尾矿的资源化利用。
Abstract:Graphene showns promising prospects due to its unique structural characteristics and excellent physicochemical properties. In this paper, graphite tailings in Luobei were taken as the research object, and graphite nano/microsheets were extracted from graphite tailings by grinding, ultrasound and gravitational settlement, followed by purification and exfoliation to prepare graphene. The results showed that the tailings particles with d50 of about 2.5µm were obtained by grinding, ultrasonic stripping was performed for 6 min, and the graphite was enriched by gravitational settlement. The yield of recycled graphite microsheets was 9.72%, and the recovery rate was 80%. After purification, graphite nano/microsheets were obtained with fixed carbon content of 98.1% and about 20 layers. Finally, the high pressure microjet homogenizer was used to exfoliate and prepare multi−layer graphene. The ratio of graphite nano/microsheets, water and dispersant was 0.2 mg∶1 mL∶0.001 mg, and the pressure of the high pressure microjet homogenizer was 80 Mpa. After 25 high−pressure dispersion cycles, the thickness of the graphene sheets was less than 10 layers and the diameter of the sheets was more than 3 μm to produce graphene with high crystal quality. The preparation of graphene from graphite tailings not only expands the range of graphene raw materials but also realizes the resource utilization of graphite tailings.
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表 1 石墨尾矿化学成分
Table 1. Chemical composition of graphite tailings
/% 元素 SiO2 Fe3O4 FeS Al2O3 K2O Na2O CaO MgO TiO2 C 含量 60.36 5.15 3.28 11.92 2.64 0.47 7.10 0.50 0.04 2.21 
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表 2 相同静置时间5 min对过渡层产率、碳含量及石墨微片回收率影响
Table 2. Effect of the same rest time 5 min on transition layer yield, carbon content and graphite sheet yield
超声时间/min 沉降产率/% 固定碳含量/% 石墨微片回收率/% 0 10.31 8.68 40.52 2 14.33 9.30 60.33 4 15.62 9.67 68.39 6 18.19 9.72 80.01 8 18.79 9.41 80.02 10 18.91 9.47 80.13
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