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二苯胺类抗氧剂合成工艺分析-analysis of synthesis technology of diphenylamine antioxidant
StudyonSynthesisofDiphenylamineAntioxidantsABSTRACTDiphenylamineantioxidantshavethefeatureswhichareownedbynotonlyamineantioxidantsbutalsophenolicantioxidants.Forexampleamineantioxidantshavethecharacteristicsofprotectingrubberproductsfromheat-resistant、oxygen、ozone、anti-fatiguecracking,atthesametime,phenolicantioxidantsarelesscontaminative、poisonousornon-toxic.Asaclassofenvironmentalantioxidants,diphenylamineantioxidantshavetakengeneralattention.Atpresent,mostofthediphenylamineantioxidantsproductedbydomesticmanufacturesaresynthesizedbydiphenylamineandolefinthroughalkylationreaction.Comparedwithsimilarforeignproducts,theeffectivecontentisless.Therefore,ithasimportantapplicationvaluetostudyandoptimizethesynthesisofdiphenylamineantioxidants.Thispaperhasreviewedthecurrentdevelopmentofrubberantioxidantsandresearchedtherepresentativeproductsofdiphenylamineantioxidantse.g.antioxidant445、antioxidantODA.Atlast,wegotabetterconditions.Inthestudy,weusedthecatalystmadebyourselftosynthesizeantioxidant445withoutorganicsolvents,andhadgotthebestsynthesisparameters:themolarratioofa-methylstyreneanddiphenylaminewas2.8:1,themasspercentageofcatalystanddiphenylaminewas16%,thereactiontemperaturewas140℃,thereactiontimewas2hours.Theproductswasrecrystallizedwithpetroleumether,andtheyieldwas95.1%.Atthesametime,wealsoexploredthemethodofcatalystregeneration.Comparedwiththeprevioussynthetsisroute,theyieldroseandtheprocesswasmoreenvironmentallyfriendly.IntheexperimentwehaduseddiisobutyleneanddiphenylaminetosynthesizetheantioxidantODAandhadgotthebestsynthesisparameters:themolarratioofdiisobutyleneanddiphenylaminewas3.2:1,themolarratioofcatalystanddiphenylaminewas1:7,thereactiontemperaturewas135℃,thereactiontimewas6hours.Afterthereaction,theproductwaswashedanddried,thefinalyieldofproductwas87%.Thissynthesismethodhadadvantagesofsafety、midnessandsoon.Keywords:diphenylamine;antioxidant445;antioxidantODA;a-methylstyrene;Diisobutylene致谢本论文在尊敬的陈天云导师的亲切关怀和悉心指导下得以顺利完成,在此谨向他表示诚挚的谢意!感谢他在我论文期间对我的实验课题顺利进行倾注了大量心
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