3,4-二氯苯基異氰酸酯連續化生產工藝研發
作者 王緒根
導師 譚心舜,論文學位 碩士,論文專業 化學工程
單位 青島科技大學

關鍵詞　3,4-二氯苯基異氰酸酯;光氣;反應器;反應動力學

摘要　3,4-二氯苯基異氰酸酯(3,4-DCPI)是重要的有機反應中間體,產品主要用于脲類除草劑、農藥合成和某些醫藥合成的中間體。近年由于需求量的增大,急需建立大規模連續化生產裝置。本文結合實際情況,通過流程模擬和小試,設計出100噸/年中試生產裝置,對中試裝置進行安裝和調試后,進行了中試,并對異氰酸酯反應動力學進行了研究。 首先,通過查閱文獻和實際情況,制定了3,4-二氯苯基異氰酸酯連續化生產的流程:將3,4-二氯苯胺用甲苯溶解,然后將液體光氣和3,4-二氯苯胺溶液通入冷反應器,再逐次經過熱反應器1、2、3后,流入光化液儲罐;確定了生產的主要約束條件和操作條件:系統負荷、光氣配比、溶劑配比、系統壓力、各反應器的溫度和攪拌轉速。通過ASPEN和PROⅡ軟件模擬,并結合實際情況設計出了3,4-二氯苯基異氰酸酯的100噸/年連續化中試生產裝置。 然后,在3,4-二氯苯基異氰酸酯中試生產裝置各個設備制造出來后,進行設備安裝和調試。在設備調試好之后,先用純溶劑在擬定條件下進行試車操作。之后,進行了不同操作條件下中試試驗。 最后,通過對中試試驗結果的整理和分析,可認定3,4-二氯苯基異氰酸酯的連續化生產完全可行。并通過中試找到了3,4-二氯苯基異氰酸酯連續化生產的較優操作條件:在系統壓力(表壓)10～20KPa;系統負荷為3,4-二氯苯基異氰酸酯150噸/年;冷反應器溫度30～40℃,冷反應器攪拌轉速750轉/分;第一熱反應器溫度80℃,第一熱反應器攪拌轉速200轉/分;第二熱反應器溫度90～100℃,第二熱反應器轉速150轉/分;第三熱反應器溫度120℃,第三熱反應器攪拌轉速100轉/分時,裝置運行良好。并進行了異氰酸酯反應動力學的研究。

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