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1、河北工业大学硕士学位论文阻燃剂四溴双酚A的合成研究姓名：李春英申请学位级别：硕士专业：应用化学指导教师：李效军20080301河北工业大学硕士学位论文熟化温度为80℃，熟化时间为60min。在此条件下母液循环三次产品质量稳定，产品收率大于91.0%，含量在98.9%以上，熔点在178.0℃~182.5℃之间。另外，本文采用连续法合成了四溴双酚A，并初步优化了合成工艺。其适宜的工艺条件为：n(双酚A):n(溴素):n(双氧水)=1:2.1:2.15，反应温度T=60℃，停留时间τ=40min，熟化时间为60min,熟化温度为回流温度(94℃)。在此条件下，产品收率为95%以上，熔点在178℃~
2、182℃之间。关键词：四溴双酚A，双酚A，溴素，双氧水，溶剂，连续法iii阻燃剂四溴双酚A的合成研究STUDYONTHESYNTHESISOFFLAMERETARDANTTETRABROMOBISPHENOL-AABSTRACTTetrabromobisphenol-Aisanexcellentflameretardant,thusthereaserchonthesynthesisoftetrabromobisphenol-Aisofgreatsignificance.Solventisoneofthemostimportantfactorsmayimpactedtheyield,melti
3、ng-points,theappearanceoftheproductandthetecnics,asaresult,thereaserchonsolvetsisalwaystheemphesisofreseach.Inthispaper,tetrabromobisphenol-Awassynthesizedfrombisphenol-A,bromine,hydrogenperoxidebyin-situbromination-oxidation,withfattyalcohols,chlorobenzene,nitrobenzene,hexamethylene,aceticacid,chl
4、orobenzene-alchols,hexamethylene-alcholsastheorganicsolvents,atthesametimetheeffectsofthesolventsonthereactionwerereasearched.Inthispaper,wetriedtosynthesizetetrabromobisphenol-Awith1-octanolasorganicsolvent.Theoptimalconditionsforthereactionwereasfollows:n(bisphenol-A):n(bromine):n(hydrogenperoxid
5、e)was1:2.05:2.1,thereactiontemperaturewasat25℃,theagingconditionwasat80℃for60min,V(1-octanol):V(water)was4:1,andthetotalvolumeofsolventwas110mlwhenthemountofbisphenol-Awas28.5g.TheyieldoftetrabromobisphenolAbasedonbisphenolAwasmorethan98.4%andthemeltingpointwasbetween178.0℃to181.3℃undertheoptimalco
6、nditionwhileusingrecycledsolvent.Inthispaper,otheralcoholswerealsousedasorganicsolventstosynthesizetetrabromobisphenol-A,theoptimalmoleculercularratiowasstudiedespeciallyandthequalityoftheproductsreachedtheappliedstandard.Inthispaper,theaceticacidwasusedastheorganicsolventtosynthesizetetrabromo-bis
7、phenol-A.Theoptimalconditionsforthereactionwereasfollows:n(bisphenol-A):n(bromine):n(hydrogenperoxide)was1:2.06:2.10,adding-timeofbromineandhydrogenperoxidewere35minrespectively,V(acticacid):V(water)=9:1and
