3,4-二氯苯基异氰酸酯连续化生产工艺研发
作者 王绪根
导师 谭心舜,论文学位 硕士,论文专业 化学工程
单位 青岛科技大学

关键词　3,4-二氯苯基异氰酸酯;光气;反应器;反应动力学

摘要　3,4-二氯苯基异氰酸酯(3,4-DCPI)是重要的有机反应中间体,产品主要用于脲类除草剂、农药合成和某些医药合成的中间体。近年由于需求量的增大,急需建立大规模连续化生产装置。本文结合实际情况,通过流程模拟和小试,设计出100吨/年中试生产装置,对中试装置进行安装和调试后,进行了中试,并对异氰酸酯反应动力学进行了研究。 首先,通过查阅文献和实际情况,制定了3,4-二氯苯基异氰酸酯连续化生产的流程:将3,4-二氯苯胺用甲苯溶解,然后将液体光气和3,4-二氯苯胺溶液通入冷反应器,再逐次经过热反应器1、2、3后,流入光化液储罐;确定了生产的主要约束条件和操作条件:系统负荷、光气配比、溶剂配比、系统压力、各反应器的温度和搅拌转速。通过ASPEN和PROⅡ软件模拟,并结合实际情况设计出了3,4-二氯苯基异氰酸酯的100吨/年连续化中试生产装置。 然后,在3,4-二氯苯基异氰酸酯中试生产装置各个设备制造出来后,进行设备安装和调试。在设备调试好之后,先用纯溶剂在拟定条件下进行试车操作。之后,进行了不同操作条件下中试试验。 最后,通过对中试试验结果的整理和分析,可认定3,4-二氯苯基异氰酸酯的连续化生产完全可行。并通过中试找到了3,4-二氯苯基异氰酸酯连续化生产的较优操作条件:在系统压力(表压)10～20KPa;系统负荷为3,4-二氯苯基异氰酸酯150吨/年;冷反应器温度30～40℃,冷反应器搅拌转速750转/分;第一热反应器温度80℃,第一热反应器搅拌转速200转/分;第二热反应器温度90～100℃,第二热反应器转速150转/分;第三热反应器温度120℃,第三热反应器搅拌转速100转/分时,装置运行良好。并进行了异氰酸酯反应动力学的研究。

The Continuously Craft Research of 3,4-Dichlorophenyl Isocyanate

keywords: 3,4-dichlorophenylisocyanate; phosgene; reactor; reaction kinetics

abstract:: 3,4-Dichlorophenyl Isocyanate(3,4-DCPI) is the important organic reaction intermediate that mainly used in the urea class weed killer, pesticidesynthesis and certain medicine syntheses intermediates. Recent years because of increasing demand, establishment large-scale continuously craft is the urgent need. This article unifies the actual situation, and slightly tries through the flow simulation, to design 100 tons/year experimental equipment, carries on the and debugs the equipment after the experimental installment, has carried on experimental, and has conducted the research to the isocyanogen diethylene glycol dinitrate reaction kinetics.First, through the consult literature and the actual situation, formulated 3,4 -phenyl-dichloride bases isocyanogen diethylene glycol dinitrate continuously to melt the production the flow: 3, 4 - dichloraniline dissolve with the toluene, the liquid carbonyl chloride and 3, 4 - dichloraniline solutions passes over the cold reactor,then gradually passes through thermal response 1, 2, 3, inflow actinic fluid storage tank; Has determined the production main restraint condition and the operating condition: The system load, the carbonyl chloride allocated proportion, the solvent allocated proportion, the system pressure, various reactors temperature and stirs the rotational speed. Through ASPEN and PROII software simulating, and the union actual situation design the continuously experimental equipment of 3, 4 - Dichlorophenyl Isocyanate for 100 tons/years.Then,afeter the continuously experimental equipment of 3, 4 - Dichlorophenyl Isocyanate has been made, carries on the equipment setup and the debugging. Debugs the equipment, first run operation using the pure solvent in to equipment under the condition to carry on the test. Afterwards, has carried on under the different operating condition.Finally, through to the experimental test result reorganization and analysis, may recognize the continuously experimental equipment of 3, 4 - Dichlorophenyl Isocyanate continuously craft to be completely feasible. And through experiment have found the more superior operating condition of the continuously craft:(table presses) 10~20KPa in the system pressure. The system load of 3 , 4-Dichlorophenyl Isocyanate is 150 tons/years. The cold reactor temperature 30~40℃. The rotational speed of the cold reactor stirs is 750 r/min. the first thermal response temperature 80 °C. The rotational speed of first thermal response stirs is 200r/min. Second thermal response temperature is 90~100℃, The rotational speed of second thermal response