十溴二苯醚催化合成及精制工藝和工藝條件優(yōu)化研究;乙嘧硫磷合成初步研究.pdf

1、湖南大學(xué)碩士學(xué)位論文十溴二苯醚催化合成及精制工藝和工藝條件優(yōu)化研究乙嘧硫磷合成初步研究姓名：楊澤慧申請(qǐng)學(xué)位級(jí)別：碩士專業(yè)：應(yīng)用化學(xué)指導(dǎo)教師：陳聲宗江多階2002.1.1湖南大學(xué)碩士學(xué)位論文AbstractThispaperstudiedtwonewprocessesforcatalyticsynthesisofdecabromodiphenyletherwhichwerecarriedoutdistinguishinglybybromi

2、natingdiphenyloxidewithbromineandbrominechlorideinthepresenceofanovelmetalcatalystUniforilltestdesignandsimplexoptimizationwereappliedintheresearch，byWhichtheoptimumreactionconditionswereobtainedAndanewmethodofDBDPOpurif

3、icationwasdevelopedTheresearchdemonstratedthatthenovelmetalcatalysthadallexcellentcatalyticperformance，suchashighcatalyticactivityhighcatalyticselectivitycomparedtOthoseoftraditionalonessuchasaluminumtrichlprideandalumin

4、umtribromidewhichweredeliquescent，hygroscopicandunstoragibleStudiesshowedthatthenoveImetalcatalystwasmoreconvenienttobeusedAsabrominatingagent，brominechloridehadhighercatalyticactivityandselectivitythanbromineFurthermore

5、theutilizationemciencyofbromineWaSimprovedbyusingbrominechloridebecausethebyproductwashydrochlgridenothydrobromideTheinfluentialfactorsofbrominatingreactionwereinvestigatedbyuniformtestandtheoptimumprocessconditionswereo

6、btainedbvsimplexoptimizationasfollows：TheoptimumreactionconditionsforcatalyticsynthesisofDBDPObybrominatingdiphenyloxidewithbrominechloridefollowedas：molarratioofdiphenylethertobrominechloridewas1：l3ratioofmetalcatalystt

7、odiphenyloxidewas1：10(w／w)diphenyletherfeedingtemperature12℃andrefluxtime72hourstheyieldofpurifiedDBDPOwasu口to971％TheoptimumreactionconditionsofcatalyticsynthesisofDBDP0bybrominatingdiphenyloxidewithbrominefoUowedas：mola

8、rratioofdiphenyIethertobrominewasl：30，ratioofmetalcatalysttodiphenyloxidewas1：5(w／w)，diphenyletherfeedingtemperature30“C，ratioofdichloromethanetodiphenyoxidewas5：lfv／v)andrefluxtime55hours，theyieldofpurifiedDBDP0wasupto9

9、52％AsimplemadconvenientDBDPOpurificationmethodWhichappliedxyleneassolventafterDBDP0hadbeenwashedwithchloroforrnwasdevelopedThenthefreebromineinthesolutionreactedwithanalkaliaqueoussolutionTheresultingsolutionwasseparated

10、andtheupersolutionwasdistilledunderareducedpressuretOremoveitssolventThusthewhitepurifiedDBDPOWaSobtainedwiththebrominecontent83l％mp：304～309℃Keywords：brominechloridebrominediphenyloxidedecabromodiphenylethermetalcatalyst