N-[(3,4,5-三氟)苯基]丙烯酰胺的合成及溶解度测定  

Synthesis and Solubility Determination of N-[(3,4,5-trifluorine)phenyl]Acrylamide

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作  者:姚新鼎[1,2] 方瑞娜 庞宏建[1,2] 刘伟 马金菊[2] YAO Xin-ding;FANG Rui-na;PANG Hong-jian;LIU Wei;MA Jin-ju(Environment Engineering Department,Yellow River Conservancy Technical Institute,Kaifeng 475004,China;Henan Engineering Technology Research Center of Green Coating Materials,Kaifeng 475004,China)

机构地区:[1]黄河水利职业技术学院环境工程学院,河南开封475004 [2]河南省绿色涂层材料工程技术研究中心,河南开封475004

出  处:《塑料工业》2021年第1期22-25,120,共5页China Plastics Industry

基  金:开封市科技攻关计划项目(1901021);河南省高等学校重点科研项目计划(20A530004)。

摘  要:以3,4,5-三氟苯胺和丙烯酰氯为原料,碳酸氢钠为缚酸剂,制得N-[(3,4,5-三氟)苯基]丙烯酰胺(TFPA)。用红外光谱、核磁共振氢谱和核磁共振碳谱对TFPA进行结构表征。探讨原料物质的量比、碳酸氢钠用量、反应温度、反应时间对TFPA收率的影响。获得适宜反应条件为:3,4,5-三氟苯胺和丙烯酰氯物质的量比为1∶1.1,碳酸氢钠为总投料质量的1.2%,反应时间5 h,反应温度5℃,产物收率可达74.4%。得到TFPA在乙醇溶剂中溶解度随温度的函数方程,拟合关联度为0.999。建立的溶解度随温度关联模型为TFPA结晶工艺提供理论指导。Taking 3,4,5-trifluoroaniline and acryloyl chloride as raw material and sodium bicarbonate as acid-binding agent,N-[(3,4,5-trifluorine)phenyl]acrylamide(TFPA)was synthesized.The chemical structure of product was characterized by means of Fourier transform infrared spectroscopy(FTIR),nuclear magnetic resonance hydrogen spectrum(1 H NMR),nuclear magnetic resonance carbon spectrum(13 C NMR).The effects of material mole ratios,sodium bicarbonate contents,reaction temperature and reaction time on the yield of TFPA were investigated.When the mole ratio of 3,4,5-trifluoroaniline and acryloyl chloride is 1∶1.1,sodium bicarbonate usage is 1.2%of the total feed mass,reaction time is 5 h and reaction temperature is 5℃,the production yield is 74.4%and the best product could be obtained.The function equation of TFPA solubility with temperature in ethanol solvent is obtained,and the fitting correlation is 0.999.The established temperature dependence model of solubility provides theoretical guidance for TFPA purification process.

关 键 词:N-[(3 4 5-三氟)苯基]丙烯酰胺 丙烯酰氯 酰胺化 溶解度关联 

分 类 号:TQ323.6􀆰[化学工程—合成树脂塑料工业]

 

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