连续法合成二氧化硫脲的管式工艺研究

3262005JOURNALOFBEIJINGUNIVERSITYOFCHEMICALTECHNOLOGYVol.32,No.620053(,100029):,,,80%,99%:;;;:TQ218:2004212201:,1978,3E2mail:[e-mail](ThioureaDioxideTD),,,[123],,,536kJ/mol[4];[5],,(3h),[627],,,1111,(1)TDCS(01185nm)CS(01181nm),,CS,TD[8],pH,,TD112(01315g,202617g),TD,,,,,,,,;,,,11Fig.1Flowsketchofexperimentalset2up113,;30%,,;BT012YZ1515();DTY28A();UV22100()114,1;23,4,5,6,8,79,10,1123040min,,,55,,,115[9];ZBG130032902211,,,,,1,,10;10%,30%;211TDTable1EffectoffeedrateonyieldandpurityofTD/(mL/min)TD/%TD/%45506515951255731396186078169719657414971170701295131,45mL/min,TD,;60mL/min,TDTD,,,,;,,,,TD212,TD,TD;,,,TD,01060mL/min10%2,TD,22,20%TD,9911%196:,,,,2,20%30%,TD,,,,TD;10%,TD,20%10%,,,,2TDTable2EffectofH2O2concentrationonyieldandqualityofTD/%TD/%TD/%/%3078169717011625791898160113208112991101111580179819011110791499100110213,pH2,,;pH614,TD,,,,,,pH26,,,01060mL/min10%20%,2,TD,33Table3EffectofquantityofNH4HCO3onreactionperformance/%pHTD/%TD/%0281139816422158214981852153831699106348415991374831098193,,,TD,5%6%,pH2154,,pH,TD3,,:0102,60mL/min;10%,20%;5%6%,80%,TD99%,[1],.[J].,2004,25(2):28-29[2],,,.[J].,2000,18(4):23-26[3].[J].,2000,7(1):30-32[4],,,.[J].,1996,22(2):206-210[5],,,.[J].,2002,43(4):39-41[6].[J].,2003,2(3):216-219[7],.[J].,1993,19(2):244-248[8],,,.[J].,1993,(2):243-248[9],.[J].,1998,27(10):759-761292005Continuoussynthesisofthioureadioxidewithapipe2stylereactorZHAOPei2yueCHENXiao2chunWUXin2yingSUNWeiLIUShi2weiYUANYin2shiLIUHu(CollegeofChemicalEngineering,BeijingUniversityofChemicalTechnology,Beijing100029,China)Abstract:Thebatchsynthesisofthioureadioxide(TD)inanaqueoussolventwaschangedtoacontinuouspipe2styleprocessinthispaper.Theinfluencesofthefeedrateoftherawmaterials,reactantconcentrationandthequantityofthepromoter,ammoniumbicarbonateontheperformanceofTDsynthesiswereinvestigated.Throughexperimentalstudy,thesuitablereactionconditionssuchasthereactiontemperature,rawmaterialra2tio,reactiontime,reactantconcentration,etc.wereobtained.Underthesuitableconditions,theyieldandpu2rityofTDproductwerehigherthan80%and99%,respectively.Keywords:thiourea;thioureadioxide;continuousreactiontechnology;pipereactor()(71)Synthesis,characterizationandstructuredeterminationofanovelLCuXcompoundscoordinatedbythe2diketiminatoligand[L=Et2NCH2CH2NC(Me)CHC(Me)O,X=Cl]ZHAOQingCAOWei2liangYANGZuo2yingZHANGJing2chang(CollegeofScience,BeijingUniversityofChemicalTechnology,Beijing100029,China)Abstract:AnovelLCuX[L=Et2NCH2CH2NC(Me)CHC(Me)O,X=Cl]compoundwascoordinatedbythe2diketiminatoligandandplentyofdryingCuCl2,andcharacterizedbyelementalanalysis,NMRandinfraredspectratechniques.Such2diketiminatoligandwaspreparedinatoluenesolventinlightofthetheoryofco2boil2ingofoilandwater.ThegeometriesoftheligandandthecomplexwereoptimizedintermsoftheDFTmethod,aLocalSpinDensityApproximationCalculations.TheIRspectrawerealsocalculatedandcomparedwiththeexperimentaldata.Andtheresultsarereasonable.Keywords:2diketiminato;N,N2diethyl2ethylenediamine;coordinationcompound;quantumchemicalcalcula2tion()396: