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1、摘要本文采用S.B技術(shù)合成了兩種芳香族酰胺化合物。對(duì)反應(yīng)條件進(jìn)行了探索和優(yōu)化.著重考察了反應(yīng)的溫度、反應(yīng)時(shí)間、反應(yīng)的初始溫度和升溫速度、芳酰氯的滴加速度、溶劑用量、反應(yīng)物的物料配比等因素對(duì)反應(yīng)的影響,以尋求最佳的反應(yīng)條件和合成工藝.將合成產(chǎn)物酰胺A和酰胺B用于聚合物的成核劑,并對(duì)其成核效果進(jìn)行了測(cè)試.本文以芳香族酰氯和脂肪族伯胺為原料,來制備芳香族酰胺化合物.產(chǎn)率可達(dá)到98%.實(shí)驗(yàn)結(jié)果表明,適當(dāng)延長反應(yīng)時(shí)間可提高產(chǎn)率.反應(yīng)的初始溫度愈高,升溫速度愈快,產(chǎn)品的收率就愈高.增加任意一種反應(yīng)物的量都可提高產(chǎn)率,但酰氯過量較胺過量來說,產(chǎn)品收率
2、的增加更為明顯.適當(dāng)提高反應(yīng)溫度,可提高產(chǎn)率.本反應(yīng)采取將一種反應(yīng)物酰氯滴加到另一種反應(yīng)物胺中的實(shí)驗(yàn)方法.酰氯的滴加速度愈慢,產(chǎn)品的收率就愈高.溶劑的使用量在不影響反應(yīng)結(jié)果的情況下,應(yīng)愈少愈好.可用DMSO作為重結(jié)晶溶劑對(duì)酰胺A進(jìn)行重結(jié)晶.收率在76.78%.溶劑的循環(huán)使用不會(huì)影響產(chǎn)品的收率.但由于時(shí)間關(guān)系,對(duì)溶劑回收精制和循環(huán)使用的次數(shù)較少。宴驗(yàn)數(shù)據(jù)還不夠充分.合成產(chǎn)物酰胺A和酰胺B可以用作飽和聚烯烴的成核劑.我們使用差示掃描量熱法和偏光顯微鏡表征成核劑對(duì)飽和聚烯烴的成核效果.結(jié)果表明:該成核劑的加入均使結(jié)晶溫度升高,結(jié)晶速度加快.并
3、使結(jié)晶的尺寸細(xì)化,結(jié)晶規(guī)整均勻,從而使結(jié)晶度增大.關(guān)鍵詞:酰胺;合成;溶劑回收;聚烯烴;成核劑ABSTRACTInthispaper,twotriamineswerepreparedbYaSchotten·Baumanreaction.Theinfluenceofreactiontemperature,reactiontime,ratioofreactantsandtheamountofthesolventwerestudiedinordertOfindtheoptimaltechnologicalconditions.Theprocu
4、ctwaspurifiedbyrecrystallizition.SynthesizeproductthetriamineAandtriamineBcanbeused弱nucleatingagentofpolyolefinandobservethenucleatingeffectofthenucleatingagent..TrimineswerepreparedwitharomaticacylchlorideandaliphaticamidebyaSchotten-Baurnanreaction.Theproductratiocallr
5、each98%.Theresultofexperimentsshowed,Proprietyextendingofreactiontimewillimprovetheyieldoftheproduct,Thebeginningtemperatureofthereactionwillleadtohi曲yield.Increasingtheamountofanyofthetworeactantswillincreasetheproductratio.Butmoreacylchloridemakesmoreproduct.Relevancei
6、ncreasingofreactiontemperaturewillincreasetheproductratio.Inthisreaction,acyIchloridewasdroppedslowlyintoamine.ThesloweracyIchloridedropped,thehighertheyieldwillbe.Thefewerconsumptionofthesolvent,thehighertheproductionratiowillbecome.DMSOWasusedasrecrystalsolventtOamideA
7、andgetayieldof76·78%.Therecycletimesofthesolventwillnotaffecttheproductratio.Asaresultofnotenoughtime,thereclaiming,refiningandrecyclingtimesofthesolventarenotenough,andtheexperimentdataarenotsufficiency.SynthesizeproductthetriamineAandtriamineBCanbeusedasnucleatingagent
8、ofpolyolefin.Differentialscanningcalorimetry(DSC)andpolarizedopticalmicroscopyWereusedtoobservethenucle