阻燃和导电可膨胀石墨的制备与性能研究

发布时间：2018-11-26 07:44

【摘要】：为了制备出用于膨胀阻燃体系的可膨胀石墨和导电防腐涂料体系的纳米石墨薄片,本文研究了以H_2SO_4/H_3PO_4、HClO_4/H_3PO_4两种混合酸,氧化插层法制备阻燃可膨胀石墨的工艺,探讨了制备工艺各因素对可膨胀石墨性能的影响,并通过正交实验法优选了可膨胀石墨的最优制备工艺;用HClO_4/H_3PO_4混合酸氧化插层和超声剥分法研究了导电纳米石墨薄片的制备工艺,得出工艺各因素对组织结构与导电性能影响作用。采用扫描电镜、X-射线衍射、激光粒度仪、原子力显微镜技术对优化工艺制备的可膨胀石墨和纳米石墨薄片进行结构形貌表征。实验结果表明:1.以H_2SO_4/H_3PO_4混酸制备的阻燃可膨胀石墨,在反应温度35℃,反应时间60 min,C(g):H_2SO_4(mL):H_3PO_4(mL):K_2Cr_2O_7(g)=1:2:2:0.12的条件下,制备出可膨胀石墨的膨胀容积为223 mL/g。添加5 g的该可膨胀石墨可以使EPS的氧指数由18%提高到26.3%。2.以HClO_4/H_3PO_4混酸制备的阻燃可膨胀石墨,在反应温度35℃,反应时间80 min,C(g):HClO_4(mL):H_3PO_4(mL):KMnO_4(g)=1:3:2:0.1的条件下,制备出可膨胀石墨的膨胀容积为235 mL/g。添加5 g的该可膨胀石墨可以使EPS的氧指数由18%提高到22.7%。3.采用微波膨胀法制备膨胀石墨,当微波功率350 W,微波时间15 s时,得到的膨胀容积为360 mL/g。与高温膨胀法相比,膨胀容积大且孔径更加密集、均匀。4.纳米石墨薄片的最佳剥分条件为:乙醇(g):膨胀石墨(g)=150:1,超声功率为400 W,超声时间为4 h~6 h,得到的纳米石墨薄片具有较大的径厚比,其平均粒度范围在17μm~10μm之间,厚度范围在50 nm~150 nm之间。添加到环氧树脂E51涂料中,当纳米石墨薄片的质量含量为20%时,涂料的体积电阻率为320Ω·cm。
[Abstract]:In order to prepare expandable graphite for intumescent flame retardant system and nano-graphite sheet for conductive anticorrosive coating system, this paper studied two kinds of mixed acids, H2SO4 / H3PO4 / HClOSP 4. The process of preparing flame retardant and expandable graphite by oxidation intercalation method was discussed. The influence of various factors on the properties of expandable graphite was discussed, and the optimum preparation process of expandable graphite was selected by orthogonal experiment. The preparation process of conductive nano-graphite sheet was studied by HClO_4/H_3PO_4 mixed acid oxidation intercalation and ultrasonic stripping method. Scanning electron microscopy (SEM), X-ray diffraction (XRD), laser particle size analyzer (LGA) and atomic force microscopy (AFM) were used to characterize the structure and morphology of the expandable graphite and nano-graphite wafer prepared by the optimized technology. The experimental results show that: 1. Flame retardant intumescent graphite prepared from H_2SO_4/H_3PO_4 mixed acid at 35 鈩，

本文编号：2357833