中国安全科学学报 ›› 2019, Vol. 29 ›› Issue (3): 127-132.doi: 10.16265/j.cnki.issn1003-3033.2019.03.021

• 安全工程技术科学 • 上一篇    下一篇

氧化石墨烯制备工艺危险性研究

周宇, 苏磊, 谢传欣** 教授   

  1. 青岛科技大学 环境与安全工程学院,山东 青岛 266044
  • 收稿日期:2018-12-16 修回日期:2019-02-28 发布日期:2020-11-26
  • 通讯作者: **谢传欣(1973—),男,安徽淮北人,博士,教授,主要从事化工过程安全方面的研究。E-mail:47566954@qq.com。
  • 作者简介:周 宇 (1993—),男,甘肃张掖人,硕士研究生,研究方向为化工过程安全。E-mail: zhouyu_904291965@qq.com。
  • 基金资助:
    国家重点研发计划专项资助(2017YFC0804801)。

Study on danger in graphene oxide preparation process based on reaction calorimetry

ZHOU Yu, SU Lei, XIE Chuanxin   

  1. School of Environmental and Safety Engineering,Qingdao University of Science and Technology, Qingdao Shandong 266044,China
  • Received:2018-12-16 Revised:2019-02-28 Published:2020-11-26

摘要: 为降低氧化石墨烯制备过程中的工艺危险性,利用反应量热仪(RC)、差示扫描量热仪(DSC)、扫描电子显微镜(SEM)、能谱仪(EDS)等仪器,探究工艺过程放热原因,测试影响热量释放的搅拌速度、加料时间、投料温度和中温阶段反应温度等参数;然后设计正交试验,得到不同条件下相关动力学参数;最后根据动力学参数正交分析,获得制备过程的最优条件。研究结果表明:放热原因是高锰酸钾的生成集聚及其快速分解。中温阶段反应温度是控制氧化石墨烯制备工艺过程危险性的重要因素。搅拌速度为250 r/min、加料时间为60 min、投料温度为0 ℃和中温阶段反应温度为20 ℃时的工况,为最优工况。

关键词: 氧化石墨烯, 反应量热仪(RC), 差示扫描量热仪(DSC), 工艺危险性, 扫描电子显微镜(SEM), 能谱仪(EDS)

Abstract: In order to reduce the risk in the preparation process of graphene oxide, experiment were carried out. RC, DSC, SEM, EDS and other instruments were used to explore the cause of heat release during the process and study effects of the stirring speed, the feeding time, the feeding temperature and the reaction temperature in the middle temperature stage and other parameters on the heat release. Orthogonal tests were designed and performed to obtain the relevant kinetic parameters under different conditions. Finally, according to the orthogonal analysis of the kinetic parameters, optimal conditions for the preparation process were obtained. The results show that the exothermic cause is accumulation and rapid decomposition of potassium permanganate, that the reaction temperature in the middle temperature stage is an important factor in controlling the risk in the process of preparing graphene oxide, and that a operating condition having a stirring speed of 250 r/min, a feeding time of 60 min, a feeding temperature of 0 ℃, and a reaction temperature of 20 ℃ in the intermediate temperature stage is the optimum operating condition.

Key words: graphene oxide, reaction calorimetry(RC), differential scanning calorimetry(DSC), process hazard analysis, scanning electron microscopy(SEM), energy dispersive spectrometry(EDS)

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