1,6-六亚甲基二氨基甲酸甲酯热解产物1,6-六亚甲基二异氰酸酯的分离  

Study on the separation of 1,6-hexamethylene diisocyanate from the thermal decomposition of 1,6-dicarbamate hexane

作　　者：曹俊雅[1] 于鑫 贺鹏[2] 王利国[2] 曹妍[2] 李会泉[2] Cao Junya;Yu Xin;He Peng;Wang Liguo;Cao Yan;Li Huiquan(School of Chemical and Environmental Engineering,China University of Mining and Technology(Beijing),Beijing 100083,China;CAS Key Laboratory of Green Process and Engineering,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China)

机构地区：[1]中国矿业大学(北京)化学与环境工程学院,北京100083 [2]中国科学院过程工程研究所绿色过程与工程重点实验室,北京100190

出　　处：《石油化工》2018年第10期92-97,共6页Petrochemical Technology

基　　金：国家自然科学基金项目(NSFC21476244)

摘　　要：采用分子蒸馏技术,对1,6-六亚甲基二氨基甲酸甲酯(HDC)热解液中1,6-六亚甲基二异氰酸酯(HDI)和1,6-六亚甲基单异氰酸酯(HMI)进行分离,考察了HDI的热稳定性,优化了模拟热解液的分离工艺条件,并利用~1H NMR,FTIR,GC等分析方法对分离后的产品进行表征及纯度分析。实验结果表明,在常压下,纯HDI在130～150℃保持稳定,160℃时开始聚合,且温度越高、时间越长,HDI热稳定性越差,分离温度应低于160℃;HDI分离的最优条件为:温度80℃、进料速度4 mL/min、HDI/HMI的质量比大于7.5;分离后产品HDI与商品HDI的结构相吻合,采用最优条件对真实热解液进行分离,分离后试样中的HDI纯度接近100%(w),表明分子蒸馏分离实验可以获得高纯度的HDI产品。Based on the technology of molecular distillation,the separation process of 1,6-hexamethylene diisocyanate(HDI)and 1,6-hexamethylene monoisocyanate(HMI)from the pyrolysis of 1,6-dicarbamate hexane(HDC)was studied.The thermal stability was studied and the separation conditions of simulated pyrolysis liquid using molecular distillation were optimized,and the obtained product HDI was characterized by 1H NMR,FTIR and GC.From the results,pure HDI was stable in the temperature range of 130-150℃,and became unstable when the temperature was higher than 160℃;the optimal separation condition was attained under 80℃with the feed rate 4 mL/min where the mass ratio of HDI to HMI was larger than 7.5.The structure of the HDI product from the separation process was consistent with HDI.At last,the real pyrolysis liquid mixture was separated under the optimized conditions,and the results showed that the purity of HDI could reach 100%(w)after separation,which meant that high purity HDI product could be obtained from the separation experiment using molecular distillation.

关 键 词：分子蒸馏 分离 1 6-六亚甲基二异氰酸酯 1 6-六亚甲基单异氰酸酯 

分 类 号：TQ226.6[化学工程—有机化工]