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为研究2-氨基-23,-二甲基丁酰胺氧化合成的热危险性,采用差示扫描量热仪(DSC)测试2-氨基-2,3-二甲基丁腈和2-氨基-2,3-二甲基丁酰胺的热分解情况,采用反应量热仪(RC1)研究反应温度、双氧水滴加速度和氢氧化钠用量对反应的影响。研究结果显示,2-氨基-2,3-二甲基丁腈吸热热分解温度为149.5℃2,-氨基-2,3-二甲基丁酰胺表现为吸热和放热2段分解过程,吸热和放热分解温度分别为234.4℃和456℃。反应放热速率主要为加料控制,但是,存在一定的热累积。热失控体系最高温度(MTSR)低于2-氨基-23,-二甲基丁腈和2-氨基-23,-二甲基丁酰胺的分解温度,高于体系沸腾温度,在热失控的条件下,反应体系容易导致冲料危险;在优惠的工艺条件范围内,提高反应温度,延长滴加时间,可降低反应的MTSR,提高热转化率和反应安全性。
In order to study the thermal risk of the oxidative synthesis of 2-amino-23-dimethylbutanamide, 2-amino-2,3-dimethylbutyronitrile and 2-amino- Dimethylbutanamide thermal decomposition of the situation, the use of reaction calorimeter (RC1) study of the reaction temperature, hydrogen peroxide drop and sodium hydroxide dosage on the reaction. The results showed that the endothermic thermal decomposition temperature of 2-amino-2,3-dimethylbutyronitrile was 149.5 ℃ 2, and the amino-2,3-dimethylbutanamide showed endothermic and exothermic two-stage decomposition , Endothermic and exothermic decomposition temperatures were 234.4 ℃ and 456 ℃. The rate of exothermic reaction is mainly controlled by feed, however, there is some heat accumulation. Thermal runaway system maximum temperature (MTSR) is lower than the decomposition temperature of 2-amino-23, -DMB and 2-amino-23, -DMB and higher than the system boiling temperature under conditions of thermal runaway Under the favorable process conditions, raising the reaction temperature and prolonging the dropping time can lower the MTSR of the reaction, and improve the heat conversion rate and the reaction safety.