苯甲酰肼与对硝基苯肼的热稳定性分析

In order to prevent fire even explosion accident caused by hydrazines in chemical industry,the adiabatic stability of benzoyl hydrazine and p-nitro phenyl hydrazine are tested by Accelerating Rate Calorimeter(ARC).Then pseudo-inverse matrix method is used to calculate dynamics parameters of the two samples respectively.Finally,the measured data are modified by considering of thermal inertia factor  of ARC.The results show that the initial exothermic temperature for benzoyl hydrazine is 141.16℃.with the maximum temperature being 364.50℃ and the time to maxinmm self-heating rate is 1061.11 min.But the initial exothermic temperature for p-Nitro phenyl hydrazine is 88.36℃,with the maximum temperature being 596.38℃ and the time to maximum self-heating rate is 314.67 min.It can be seen that p-nitro phenyl hydrazine is easier to explode and the explosion is more powerful.

N-(1-苯基-3-甲基-4-苯亚甲基-5-吡唑啉酮)对硝基苯甲酰肼(PMBP-PNH)的合成和晶体结构

合成了标题化合物(C24H19N5O4,Mr = 441.44),晶体属单斜晶系,P21/n空间群,晶胞参数为: a = 9.151(2) , b = 18.405(5) , c = 13.061(3) , = 101.12(1), V = 2158.5(9) 3, Z = 4, Dc = 1.358 g/cm3, = 0.096 mm-1, F(000) = 920, R = 0.0468,wR = 0.1090。分子间以氢键形成二聚体。

对硝基苯甲酰芳肼的合成及氧化脱氢研究

4-nitro benzoyl acylhydrazines are synthesized in ice bath with substituted hydrazine and 4-nitrobenzoic chloride as raw materials. At the same time ,4-nitrobenzoic acyl azo compounds are synthesized firstly with the oxidation system NBS/Pyridine. The products are characterized by elementary analysis, IR and 1HNMR, The yields of products are about from 80% to 92%.

α-(对硝基苯氧基)十四酸酰肼的合成

报道了α-(对硝基苯氧基)十四酸酰肼的合成方法。以十四酸为原料经α-(对硝基苯氧基)十四酸乙酯中间体,用水合肼肼解得到α-(对硝基苯氧基)十四酸酰肼。用乙腈-氯仿混合溶剂重结晶获得纯品,收率67.9%。通过元素分析、红外光谱及核磁共振谱确定了该化合物的结构。

对硝基苯乙酮缩水杨酰肼Schiff碱的合成与晶体结构

合成了一种新的Schiff碱对硝基苯乙酮缩水杨酰肼,进行了红外光谱、紫外光谱和元素分析表征,并且测定了该化合物的晶体结构,该晶体属于单斜晶系,P2(1)/c空间群。晶胞参数a=1.6068(3)nm,b=1.1838(2)nm,c=0.72901(15)nm,β=91.39(3)°.

1-对硝基苯基-3-甲基-4-(α-噻吩甲酰基)-5-吡唑啉酮的合成

对硝基苯肼与乙酰乙酸乙酯经亲核闭环制得1-对硝基苯基-3-甲基-5-吡唑啉酮(1);1与α-噻吩甲酰氯进行克莱森缩合合成了新化合物——1-对硝基苯基-3-甲基-4-(α-噻吩甲酰基)-5-吡唑啉酮,其结构经1H NMR,13C NMR,IR,MS和元素分析表征。

对硝基苯甲酰芳基偶氮化合物的合成及其结构表征

以取代苯肼、自制的对硝基苯甲酰氯为原料,用冰浴法合成了3种对硝基苯甲酰芳肼化合物;并用NaBrO3/H2SO4氧化体系脱氢得3种对硝基苯甲酰芳基偶氮化合物,产品的结构经元素分析、IR、1HNMR确证,产率在84%—93%之间。