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1、鏑:103082空訂1分類號:——密級:——單位代碼:學(xué)號:西北大學(xué)碩士學(xué)位論文指導(dǎo)教師:型苤盎專業(yè)技術(shù)職務(wù):副麴握學(xué)科(專業(yè)):絲堂王苧答辯日期:2007.5.25學(xué)位授予日期:二00七年五月摘要本文首先簡要介紹了無水哌嗪的市場發(fā)展情況以及相關(guān)用途。根據(jù)以乙二胺為原料常壓氣固相催化合成哌嗪的小試研究結(jié)果,依據(jù)反應(yīng)工程學(xué)的基本原理,確定了放大方法、放大準(zhǔn)則和放大參數(shù)。通過單因素實驗和正交實驗,對放大過程中的影響因素進(jìn)行了研究,校正了放大參數(shù),確定了合成無水哌嗪的最佳工藝條件。通過對催化劑的失活研究,了解了各因素對催化劑失活的影響,得出了催化劑的結(jié)焦
2、速率方程。最后以實驗相關(guān)數(shù)據(jù)為依據(jù),對建成年產(chǎn)300噸無水哌嗪的工廠作了經(jīng)濟(jì)前景預(yù)測和分析。本文為哌嗪的工業(yè)化生產(chǎn)提供了理論依據(jù)和實驗基礎(chǔ)。結(jié)果表明:1.在最優(yōu)溫度和進(jìn)料濃度條件下,維持小試最佳空速是放大準(zhǔn)則,經(jīng)校正得最佳空速為0.0187m一.g叱^r~,是基本放大參數(shù)。2.放大合成實驗所確定的最佳工藝條件為:原料液濃度40%(質(zhì)量分?jǐn)?shù)),反應(yīng)溫度360"C,反應(yīng)空速為0.0187m甜.譬.1.hr-1。在此工藝條件下,7,--胺的轉(zhuǎn)化率為96.19%,哌嗪的收率為61.985,三乙烯二胺的收率為30.735,總收率為92.71%。3.對該反應(yīng)催
3、化劑失活的研究表明該催化劑具有較好的抗結(jié)焦性,其結(jié)焦速率方程為:Vc=d(Cc%)/dt=.6E-07t2+2E.4t+o.00884.以乙二胺為原料常壓氣相法合成無水哌嗪的工藝路線是可行的,經(jīng)濟(jì)前景預(yù)測和分析表明該產(chǎn)品具有較好的經(jīng)濟(jì)效益和社會效益。關(guān)鍵詞:無水哌嚷合成工藝失活StudyonthePilotPlantSynthesisofPiperazineThepaperhasreviewedthemarketdevelopmentandrelatedUSeSofpiperazine.BasedonthepredecessorstudyOilde
4、aminationofindustrialethylenediamineonnormalpressureandonthebasicprinciplesofreactionengineerlng,themethod,criteriaandparameterofamplificationisdetermined.Thenmonofactormethodandmultifactorogthogonalizingdesignmethodareappliedtoresearchtheaffectionsofthefactors,,tOcalibratethe
5、parameter,andtogettheoptimumprocessingconditionsinpreparationofpiperazine.Bymeadsofthestudyondevitalized-catalysttogettheinfluenceofthefactorandtherateequation.Finally,theeconomicanalysisonproductionof300t/apiperazinewasmadeonthebasisoftheresultsintheexperiment.Thefollowinghav
6、ebeenobtainedthroughlotsofexperiments.1.Attheoptimalconditionsoftemperatureandfeedconcentration,maintainingthebestairspeedtestedinpredecessorstudyistheamplificationcriteria,anditis0.0187mot·94^,.-t,itisthebasicparameterofamplification.2.Theoptimumprocessingconditions:theconcen
7、trationofEDA40%(massfiaction);reactiontemperature360"C;spacevelocityO.0187mot·g-t.hr4.Intheseconditions,theconversitionofEDAIS96.19%,theyieldofPAis61.98%,theyieldofTEDAis30.73%andthetotalis92.71%.3.Thestudyofdevitalized-catalystshowsthatthecatalysthasagoodqualityonanti--cokeab
8、lity.Therateequationofcokeisasfollow:Vc=d(Cc%)/dt=.6E.0712+28