某医药中间体合成工艺的热危险性研究

【作者】 杨茜；

【导师】 陈网桦； 陈利平；

【作者基本信息】 南京理工大学 ， 安全技术及工程， 2012， 硕士

【摘要】 工厂在新工艺投产前有必要对工艺进行热风险评估,以保证安全生产。本文对某医药中间体的合成工艺进行了的热风险评估。主要通过实验室全自动反应量热仪(RCle)测试了每一步的热力学数据,同时利用差示扫描量热仪(DSC)以及AKTS高等动力学软件研究了产物的二次分解特性,从而对反应的热危险性进行评估分级。首先进行实验室小试,初步了解反应的放热特征；再采用RCle研究每一步的放热特性计算得出反应失控条件下的绝热温升(ΔTad)、反应所能达到的最高温度(MTSR)等参数；用DSC对反应产物进行扫描量热,得到产物高温下的热分解情况,用AKTS软件进行动力学模拟,根据模拟结果计算得到诱导期为24h所对应的温度TD24等参数；最后结合这些数据,根据热失控危险等级分类标准进行热失控危险等级划分。结果表明：在由3个反应构成的合成工艺中,反应2的放热量最小,几乎不放热,反应3的放热量最大,引起的绝热温升也最高,反应1居中；反应3在投料初始阶段放比较剧烈,值得注意；3个反应的热风险等级分别为三级、一级、三级,均可以接受,只需采取适当的措施就可以使合成工艺的热风险处于受控状态内。更多还原

【Abstract】 The runway reaction often leads to combustion and explosion accidents in chemical factory. It is necessary to carry out the systems analysis, testing, evaluation and investigation on the direction of security control before a new process production.In this paper, Reaction Calorimeter (RC1e), Differential Scanning Calorimeter(DSC) and Advanced Kinetics and Technology Solutions (AKTS) were used to study the thermal risk of the synthesis of a pharmaceutical intermediate. First of all, the cp of some raw materials was tested by DSC. Then some experiments were carried out with RC1e to study the exothermic character of each step. Some parameters such as adiabatic temperature increase (ΔTad), maximum temperature of synthetic reaction(MTSR) were obtained. After that DSC was used to study the thermal decomposition of each product, and some apparent parameters, such as onset temperature, heat release were obtained. On the base of DSC data, the kinetics parameters and TD24 were got with AKTS simulation. Finally combining the datum from RC1e, DSC and AKTS, the thermal risk class of each reaction is studied.The results showed that the second reaction has the minimum heat release, and the third reaction has the maximum heat release. The risk class of thermal runaway reaction of first reaction is class 3, the risk class of thermal runaway reaction of the second reaction is class 1, and the risk class of thermal runway reaction of the third reaction is class 3. The thermal risks of three reactions are all acceptable and appropriate measures should be taken to ensure the reaction under control.更多还原