硝-硫混酸硝化1,3,3-三甲基-1-苯基茚满工艺优化及反应热危险性等级评定  

Process Optimization and Thermal Hazard Rating in Nitrification of 1,3,3-Trimethyl-1-Phenylindane with Nitric Acid and Sulfuric Acid

作　　者：钟佳琪 邢泽铭 李晓雷 ZHONG Jiaqi;XING Zeming;LI Xiaolei(Shanghai Research Institute of Chemical Industry Co.,Ltd.,Shanghai 200062,China)

机构地区：[1]上海化工研究院有限公司,上海200062

出　　处：《上海塑料》2022年第4期8-12,共5页Shanghai Plastics

摘　　要：以1,3,3-三甲基-1-苯基茚满为原料,与硝-硫混酸进行硝化反应合成5(6)-硝基-1-(4-硝基苯基)-1,3,3-三甲基茚满(DNPI),用红外光谱(FTIR)和核磁共振氢谱(^(1)H-NMR)对其结构进行了表征,对硝化反应溶剂、反应时间、反应温度和物料配比进行考察。结果表明:n(1,3,3-三甲基-1-苯基茚满)∶n(硝酸)∶n(硫酸)=1.00∶2.15∶6.00,氯仿为溶剂,在25℃下反应时间3 h,DNPI的粗收率为98.6%。对优化后的工艺进行反应热安全风险测试和评估,得到硝化反应工艺的危险度等级为1级。5(6)-nitro-1-(4-nitrophenyl)-1,3,3-trimethylindane(DNPI)was synthesized from 1,3,3-trimethyl-1-phenylindane by nitration with nitric acid and sulfuric acid.Its structure was characterized by Fourier transform infrared reflection(FTIR)and nuclear magnetic resonance hydrogen spectrum(^(1)H-NMR).The reaction solvent,reaction time,reaction temperature and material ratio were investigated.The results show that the crude yield of DNPI is 98.6% when n(1,3,3-trimethyl-1-phenylindane)∶n(nitric acid)∶n(sulfuric acid)=1.00∶2.15∶6.00,chloroform is used as solvent,at 25℃ for 3 h.The optimized process is tested and evaluated for the safety risk of reaction heat,and the risk level of the nitrification reaction process is obtained as grade 1.

关 键 词：5(6)-硝基-1-(4-硝基苯基)-1 3 3-三甲基茚满 硝化 工艺优化 反应热 危险性等级 

分 类 号：TQ433.4[化学工程]