摘要
以硝酸和环己醇为原料 ,硫酸为催化剂 ,氯仿为溶剂 ,尿素和硫酸铵为混合反应稳定剂 ,合成了柴油十六烷值改进剂 -硝酸环己酯 ,在实验条件下确定了最佳合成条件。结果表明 ,以 0 .2 72mol环己醇为准 ,硫酸与硝酸的摩尔比为 2∶1,硝酸与环己醇摩尔比为 1.35∶1,混酸温度和酯化温度均为 0～ 5℃ ,在该温度下酯化反应时间为4 0～ 5 0min ,室温反应 10min ,尿素和硫酸铵分别为 0 .3g和 5 g。在此条件下 ,反应比较平稳、安全 ,得到硝酸环己酯的产率和纯度都较高。产品经密度和折光率、元素分析、红外光谱分析 。
The synthesis of cyclohexyl nitrate is presented from nitric acid and cyclohexanol with sulfuric acid as catalyst, and chloroform as solvent, and urea and (NH 4) 2SO 4 as stabilizator of the reaction. According to the experimental results, optimum conditions of synthesis of cyclohexyl nitrate were determined and developed. The result shows that the molar ratio of H 2SO 4 and HNO 3, HNO 3 and cyclohexanol is 2∶1 and 1.35∶1 respcetively, and that temperature of mixed acid and esterification are all 0～5 ℃, time of esterification is 40～50 min at 0～5 ℃ and 10 min at room temperature, and urea and (NH 4) 2SO 4 is 0.3 g and 5 g separately(based on 0.272 mol cyclohexanol). In the conditions the reaction is smooth and steady, safe and reliable, and both the yield and purity of cyclohexyl nitrate are very high. The structure of the product is identical with that of the title compound. It is confirmed by density, refractive index, elementary analysis and IR spectra.
出处
《石油化工高等学校学报》
CAS
2002年第1期18-20,共3页
Journal of Petrochemical Universities
