硼酸三丁酯的合成

20101Jan.2010CHEMICALINDUSTRYANDENGINEERING27Vol.271No.1:2009-08-04:(1986-),,,:,:[phone],E2mail:[e-mail]:1004-9533(2010)01-0007-04,,,(,102617):,():0110moln()/n()512()m(NaHSO4)/m()212%1310min8714%,()1820:;;;:O627131:ASynthesisofTributylBorateZHANGJi2chu,ZHANGHai2bo,LIUXia,ZHANGLi2fang(ChemicalEngineeringDepartment,BeijingInstituteofPetrochemicalTechnology,Beijing102617,China)Abstract:Tributylboratewassynthesizedbyesterificationofboricacidwithn2butanolundermicrowaveirradiation.Theeffectsofcatalyst,water2carryingreagent,reactiontimeandreactiontemperaturehavebeeninvestigated.Theoptimumconditionofreactionhasbeenfound:boricacid612g(0110mol),n2butanol4714mL(0152mol,alsoaswater2carryingreagent),onehydratedsodiumbisulfateascatalyst110g(212%ofthetotalmassofrawmaterials),microwaveirradiationtime1310min,theaverageyieldofproductis8714%.Thereactionundermicrowaveirradiationwasabout1820timesfasterthanthatunderconventionalheating.ThephysicalpropertyandstructureofproducthavebeencharacterizedbyIRandelementaryanalysis.Keywords:tributylborate;microwaveirradiation;esterification;synthesis,,,,,45h[14],,,,,,[57],,,201011111MAS2I/()CL22()2WA2J()FTIR2750(Nicolet)FlashEA21112()112,B(OH)3+3CH3CH2CH2CH2OHB(OCH2CH2CH2CH3)3+3H2O612g(0110mol),4714mL(0152mol),110g,250mL,5,:60210min,80210min,90510min,100210min,118210min,1310min,,,,100mL,,,8589/016kPa,2012g,8714%()2211:612g(0110mol)2714mL(0130mol)10mL1310min(60210min80210min90510min100210min118210min),4,11,,,,1Table1Effectofwater2carryingreagentontheyield/%1101678128011831480178014117178015212612g(0110mol)3714mL(0141mol,)1310min(60210min80210min90510min100210min118210min)110g,4,22Table2Effectofcatalysttypeontheyield%8312831081102,,,,,,,,213:,110g1310min(60210min80210min90510min100210min118210min)612g(0110mol),,,38271:3Table3Effectofratioofboricacidandn2butanolontheyield/mL371447145714n()/n()411512613%8310871289123,(),,n()/n()512,,,214:612g(0110mol)4714mL(0152mol)1310min(60210min80210min90510min100210min118210min),,,44Table4Effectofcatalystamountontheyield/g016110210%8318871287134,,,,,110g,212%215:612g(0110mol)4714mL(0152mol),110g,55,4,,,,1310min;65144,3(90),,90,,,,90,525Table5Effectofmicrowaveirradiationtimeontheyield12345/608090100118/min%1/min210210310210210111085142/min210210510210210131087133/min210310510210210141087134/min210510510210210161087145/min210510210210210131083146/min2105100100100107104318216,,:612g(0110mol)4714mL(0152mol)110g(212%)1310min,3,8715%8713%8714%,8714%217,,216,415h,7712%,,,193311,(n20D=11407)[1],,3,:2959cm-1(s)2870cm-11482cm-11420cm-1(s)(CH3CH2);1337cm-1(BO);12591071cm-1(CO)312(%),920101():C62162%(62104%);H11183%(12118%),41),:612g(0110mol)4714mL(0152mol,)110g(212%)1310min,8714%2),,()19:[1].()[M].:,1992[2],.[J].,1999,28(2):90-92[3],.[J].,2002,19(9):503-505,527[4],,,.[J].,2006,29(3):36-38,42[5],.[J].,2001,21(4):8-12[6],.[J].,2002,22(3):212-219[7],,,.[J].,1996,23(4):49-5201