基于扫描升温模式的差示功率补偿绝热量热方法

Differential power compensation’s adiabatic calorimetry method based on scanning heating mode

为了解决传统绝热加速量热仪反应检测效率低、反应判断灵敏度不高、绝热性能受限的问题,提出差示功率补偿绝热扫描量热方法.在实验样品分解反应的激发阶段,用扫描模式匀速升温,并采用基于扫描基线的两通道补偿功率差、温差和样品温升速率3种动态反应检测方法并行进行检测,以适应复杂工况的反应环境,提高反应检测效率和灵敏度;当判断发生反应后,结合差示功率补偿控制和基于恒温基线的动态绝热追踪,使样品实现接近理想的绝热反应过程.以过氧化二叔丁基(DTBP)为实验对象进行实验验证,结果表明,与传统绝热加速量热方法相比,差示功率补偿绝热扫描量热方法在0.3~0.7℃/min的扫描速率范围内,能明显提高反应检测效率和灵敏度,并可以得到更准确的热分解特性参数和动力学参数.

A differential power compensation adiabatic scanning calorimetry method was proposed,in order to solve the problems of low reaction detection efficiency,low reaction judgment sensitivity,and limited adiabatic performance of traditional adiabatic accelerating calorimeter.During the excitation stage of sample decomposition reaction,scanning mode is used to heat up the entire two-channel reaction system at a constant rate,and in order to adapt to the reaction environment of complex working condition,three dynamic reaction detection methods based on scanning baseline,i.e.,two-channel heating power difference,two-channel sample temperature difference,and sample temperature rise rate,are used at the same time to improve the reaction detection efficiency and sensitivity.When the reaction happens,the differential power compensation control method and the dynamic adiabatic tracking method based on the constant temperature baseline are combined,making the sample achieve close to ideal adiabatic reaction process.The experimental verification with di-tert-butyl peroxide(DTBP)as the experimental object shows that the differential power compensation adiabatic scanning calorimetry method can significantly improve the reaction detection efficiency and sensitivity,and obtain more accurate thermal decomposition characteristics and kinetic parameters within the scan rate range of 0.3℃/min to 0.7℃/min compared with traditional adiabatic accelerating calorimetry method.