文献类型：期刊文献

中文题名：重氮乙酸乙酯合成工艺过程热风险性研究

英文题名：Study on thermal risk of ethyl diazoacetate synthesis process

作者：任彦浩[1,2];叶启亮[1];马莹莹[2];袁佩青[1]

机构：[1]华东理工大学化工学院,上海200237;[2]上海索尔维投资有限公司热安全实验室,上海201100

年份：2022

卷号：51

期号：12

起止页码：3430

中文期刊名：应用化工

外文期刊名：Applied Chemical Industry

收录：CSTPCD;;北大核心:【北大核心2020】；CSCD:【CSCD_E2021_2022】；

基金：国家自然科学基金项目(22178113)。

语种：中文

中文关键词：重氮乙酸乙酯;反应量热;过程控制;风险评估;安全措施

外文关键词：ethyl diazoacetate;reaction calorimetry;process control;risk assessment;safety measures

摘要：采用了差示扫描量热仪和加速绝热扫描量热仪对重氮乙酸乙酯的相关热力学参数进行了测量,通过相关动力学分析得到了反应最大速率的到达时间(TMR ad),利用反应量热仪对重氮乙酸乙酯合成工艺进行量热实验,并通过量热数据获得了绝热温升、反应焓变和体系在失控情形下所能到达的最高合成温度(MTSR),比较合成温度(T_(p))、失控情形下到达的最高合成温度(MTSR)、二次分解温度T_(D24)以及技术原因的最高温度(MTT),确定风险级别。结果表明,重氮乙酸乙酯起始分解温度为85℃,放热量149.146 J/g,具有潜在的分解危险性;重氮化合成工艺的风险等级为:T_(p)Differential scanning calorimeter and accelerated adiabatic scanning calorimeter were used to measure the relevant thermodynamic parameters of ethyl diazoacetate.The time of arrival(TMR ad)of the maximum reaction rate was obtained through correlation kinetic analysis.The reaction calorimeter was used to conduct calorimetric experiments on the synthesis process of ethyl diazoacetate,and the adiabatic temperature rise and the reaction enthalpy change and the maximum synthesis temperature(MTSR)that the system can reach in the case of out of control,compare the synthesis temperature(T_(p)),the maximum synthesis temperature(MTSR)reached in the case of out of control,the secondary decomposition temperature T_(D24)and the maximum temperature(MTT)for technical reasons,and determine the risk level.The results show that the initial decomposition temperature of ethyl diazoacetate is 85℃,and the heat release is 149.146 J/g,which has potential decomposition risk;the risk of diazotization synthesis process is:T_(p)