环丙基甲基酮连氮的制备及物化性质  

Preparation and physicochemical properties of cyclopropyl methyl ketazine

作　　者：赵文昭 赵鹏 刘龙[1] 夏洋峰 张延强[3,4] Wenzhao ZHAO;Peng ZHAO;Long LIU;Yangfeng XIA;Yanqiang ZHANG(Beijing Key Laboratory of Ionic Liquids Clean Process,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China;School of Chemical Engineering,University of Chinese Academy of Sciences,Beijing 100049,China;Key Laboratory of Science and Technology on Particle Materials,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China;Zhengzhou Institute of Emerging Industrial Technology,Zhengzhou,Henan 450000,China)

机构地区：[1]中国科学院过程工程研究所离子液体清洁过程北京市重点实验室,北京100190 [2]中国科学院大学化学工程学院,北京100049 [3]中国科学院过程工程研究所中国科学院粉体材料技术重点实验室,北京100190 [4]郑州中科新兴产业技术研究院,河南郑州450000

出　　处：《过程工程学报》2021年第2期183-192,共10页The Chinese Journal of Process Engineering

基　　金：国家自然科学基金资助项目(编号:21878278,21676281);北京市自然科学基金资助项目(编号:2192054)。

摘　　要：以环丙基甲基酮和水合肼为原料,合成了一种新的酮连氮(环丙基甲基酮连氮)。针对所得环丙基甲基酮连氮,在测定(计算)其物化性质(密度、黏度、熔点、比热容、表面张力、分子单点能等)的基础上,进一步测定了环丙基甲基酮+环丙基甲基酮连氮二元体系的气液相平衡(VLE),并应用NRTL模型对实验数据进行了关联。结果表明,在优化的反应条件下(原料摩尔比2.0:1、温度363.2 K、压力101.3 kPa和时间7 h),环丙基甲基酮连氮产率达93.6%。Ketazines as useful intermediates have been extensively applied in many industrial fields,including dyes,pharmaceuticals,aviation fuels,photosensitive materials,as well as polymerizable monomers.In this work,a new ketazine derivative(cyclopropyl methyl ketazine,C_(10)N_(2)H_(16))was prepared from cyclopropyl methyl ketone and hydrazine hydrate.Under the atmospheric pressure,the reaction was studied under different mole ratios of cyclopropyl methyl ketone to hydrazine,reaction temperatures,and reaction times.With the optimized reaction conditions of 2.0:1,363.2 K,101.3 kPa and 7 h,the yield of cyclopropyl methyl ketazine was up to 93.6%through the chromatograph measurements.The structure of cyclopropyl methyl ketazine was characterized by IR and NMR spectra after it was purified through distillation.In order to prove the existence of isomers,Gaussian 09 program to optimize the structures was used and the energy values(single point energy)of cyclopropyl methyl ketazine was calculated.Furthermore,a comprehensive set of the physicochemical parameters for cyclopropyl methyl ketazine was provided,including density[ρ=0.884~0.947 g/cm^(3)],dynamic viscosity(η=1.39~2.88 m Pa×s),liquid heat capacity[Cp=2.03~2.32 J/(g·K)]and surface tension(σ=22.1~25.0 m N/m)in temperature range(280~400 K).The data ofρ,ηandσexhibited the negative correlations with temperature,while V_(m),αand C_(p )showed the positive correlations with temperature,which all had a good fitting degree for equations.Considering the cyclopropyl methyl ketazine reaction systems,the vapor-liquid equilibria(VLE)of binary system(cyclopropyl methyl ketone-cyclopropyl methyl ketazine)was measured and correlated with NRTL model to acquire the binary interaction parameters.The obtained data and correlations are valuable for industrial processes,and could be the good references for industrial design.

关 键 词：环丙基甲基酮连氮 物化性质 气液相平衡 异构体 

分 类 号：O623.542[理学—有机化学]