高纯石墨的制备研究.doc

高纯石墨的制备研究 王 磊 摘 要 为了改进传统的高纯石墨生产方法，找到高效环保的生产工艺，采用密闭微波消解技术对石墨进行了提纯。系统地研究了石墨样品的预处理、消解液的配比、消解压力、微波消解时间和微波消解功率对提纯效果的影响。 通过轮换实验得出了以下结论：随着HCl/HNO3比值和微波消解功率的增加产品固定碳含量先增大后减小；产品固定碳含量随着石墨原料微波预处理时间、微波消解压力和微波消解时间的增加而增加。同等反应条件下，石墨原料经微波预处理5min，取出骤冷，产品固定碳含量更高。 密闭微波消解提纯石墨的最佳实验条件：原料经过微波预处理5min后骤冷，消解液选用HCl:HNO3 ＝2:22.0Mpa，消解时间30min。制得了固定碳含量为99.449％的石墨产品。 关键词 高纯石墨，微波，提纯  ABSTRACT In order to improve the traditional methods of production of high-purity graphite and find environmentally friendly and efficient production processes, the closed microwave digestion technique had been used in purification of graphite. The Influence factor of purity such as the pretreatment of graphite samples, the ratio of liquid digestion, digestion pressure, digestion time and microwave power have been systematically studied. The result of experiment obtained by rotation experiment showed that: with the increase of the ratio of HCl/HNO3 and microwave digestion power, the content of carbon in the product increased first and then decreased; with the increase of the pretreatment time, digestion time and digestion pressure, the content of carbon increased ; in the same reaction conditions, the content of carbon is more higher as the graphite materials is dealt with by microwave pretreatment for 5min, sudden cold and then. The best experimental conditions of closed microwave digestion purification of graphite are as followed: after a microwave pre-treatment of raw materials after the first 5min，sudden cold ，digestion solution selected HCl: HNO3 = 2:2, digestion power 800W, digestion pressure 2.0Mpa, digestion time 30min. The content of carbon in the product at the best conditions is 99.449%. Key words High-purity graphite, microwave, purification  目 录 摘 要 I ABSTRACT II 目 录 1 1 绪 论 1 1.1 研究背景 1 1.2 研究现状 2 1.2.1 高碳石墨提纯工艺 2 1.2.2 微波技术加热原理 4 1.2.3 微波技术的应用 4 1.3 课题的研究内容 5 1.4 课题的目的及意义 5 2 高纯石墨制备实验 7 2.1 实验药品及仪器 7 2.1.1 实验药品 7 2.1.2 实验仪器 7 2.2 实验方案 7 2.2.1消解样