CAJ | 학술논문

利用全自动反应量热器（RC1e）测定了1，1-二氨基-2，2-二硝基乙烯（FOX-7）合成过程中的硝化反应热释放速率及传热系数、比热容。结果表明硝化反应加料过程中的平均放热速率约为80 W ，保温反应过程中的平均放热速率约为40 W ，物料放热量为375．22 kJ·mol-1，理论绝热温升为483．8 K。采用差示扫描量热法（DSC）和热重-微商热重（TG-DTG）法分析了中间体2-（二硝基亚甲基）-5，5-二硝基嘧啶-4，6-二酮的热稳定性，其分解分为两个阶段，起始分解温度为30℃，第一阶段分解峰温为67．01℃，放热量为201．2 J·g-1；第二阶段分解峰温为87．15℃，放热量为1046．6 J·g-1，表明中间体的热稳定性较差。
이용전자동반응량열기（RC1e）측정료1，1-이안기-2，2-이초기을희（FOX-7）합성과정중적초화반응열석방속솔급전열계수、비열용。결과표명초화반응가료과정중적평균방열속솔약위80 W ，보온반응과정중적평균방열속솔약위40 W ，물료방열량위375．22 kJ·mol-1，이론절열온승위483．8 K。채용차시소묘량열법（DSC）화열중-미상열중（TG-DTG）법분석료중간체2-（이초기아갑기）-5，5-이초기밀정-4，6-이동적열은정성，기분해분위량개계단，기시분해온도위30℃，제일계단분해봉온위67．01℃，방열량위201．2 J·g-1；제이계단분해봉온위87．15℃，방열량위1046．6 J·g-1，표명중간체적열은정성교차。
The thermodynamic data of heat flow curve,heat transfer coefficient and heat capacity in nitration reaction of 2-meth-ylpyrimidine-4,6-dione in the synthesis of 1,1-diamino-2,2-dinitro ethylene(FOX-7)were measured by using reaction calorimeter ( RCle). Results show that the average heat release rate of nitration reaction in feeding is about 80W and in the finishing period about 40W. The total exothermic heat of nitration reaction is 375. 22 kJ·mol-1 ,and the adiabatic temperature rise is 483. 8 K. The thermal behaviors of 2-dinitromethylene-5,5-dinitropyrimidine-4,6-dione were analyzed by differential scanning calorimeter and thermo-gravimetry-derivative thermogravimetric analysis techniques. Results show that its thermal decomposition process can be divided into two stages. The initial decomposition temperature is 30 ℃,the peak temperature of first-stage is 67. 01 ℃ and the enthalpy of decomposition reaction is 201. 2 J·g-1. The peak temperature of second-stage is 87. 15 ℃ and the enthalpy of decomposition reaction is 1046.6 J·g-1. This indicates that the thermal stability of 2-dinitromethylene-5,5-dinitropyrimidine-4,6-dione is bad.