甲基四氢苯酐合成过程研究

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甲基四氢苯酐是一种耐热、耐化学稳定及有优良的物理和电气性能并且熔点高,升华现象小,对环境影响小的环氧树脂的固化剂。为解决现有的间歇工艺流程中存在的一些不足之处,本文重点对该双烯合成反应的反应动力学各个因素进行测试分析,研究不同的溶剂、不同的浓度、不同的温度下对反应速率常数、活化能和指前因子的影响。经过对比分析,选用填料塔作为反应器,对填料塔进行初步计算分析,提出连续合成中试工艺方案的设想。实验结果表明:温度和浓度对反应有一定的影响,在合适的温度和较低的浓度下反应才比较容易控制;在不同的溶剂下得到的活化能和指前因子都不相同;低浓度的反应温度稳定得较快,放热少,易于控制,而高浓度的反应放热快而且高,不容易控制分析,且容易发生聚合反应生成聚合物,对反应不利。经过数据的对比分析,得到固化剂作溶剂的活化能Ea=8.26×104 J/mol,指前因子A=5.95×1012。 Methyl tetrahydrophthalic anhydride is a curing agent that is resistant to heat, chemically stable and has excellent physical and electrical properties, high melting point, low sublimation, and little environmental impact. In order to solve some existing deficiencies in the batch process, this paper focuses on the kinetics of the reaction of the diene reaction of various factors to test the analysis of different solvents, different concentrations, different temperatures, the reaction rate The effect of constant, activation energy and pre-exponential factors. After comparative analysis, choose the packed tower as the reactor, the packed tower for the initial calculation and analysis, put forward the idea of ​​continuous synthesis pilot process. The experimental results show that the temperature and the concentration of the reaction have a certain impact on the reaction at a suitable temperature and lower concentration was relatively easy to control; in different solvents obtained activation energy and pre-exponential factors are not the same; low concentration The reaction temperature is stable, the exotherm is less and the reaction is easy to control. However, the exothermic reaction with high concentration is fast and high. It is not easy to control the analysis, and the polymerization reaction is prone to generate the polymer, which is unfavorable to the reaction. After comparative analysis of the data, the activation energy of the curing agent as solvent Ea = 8.26 × 104 J / mol and the pre-exponential factor A = 5.95 × 1012.
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