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1、浙江大學(xué)碩士學(xué)位論文2-氰基吡嗪的合成研究姓名:翟靜申請學(xué)位級別:碩士專業(yè):化學(xué)工程指導(dǎo)教師:戴君裕2003.3.1摘要本文塒毗嗪類化合物在醫(yī)藥、農(nóng)藥、香料等領(lǐng)域中的用途進行了簡單的介紹,對H的產(chǎn)物2一氰基吡嗪研發(fā)態(tài)勢、市場時景及意義進行了論述,并綜述了2~氰旗毗嗪和2一甲基吡囔的文獻合成方法。首先以乙二股與1,2一丙二醇為原料,在固定床反應(yīng)器中反應(yīng)合成2一甲基毗嚓。用含CuO41.26%,ZnO41.79%,A12037.75%的KB-207型催化劑,分jjjj改變反應(yīng)扎矗度、原料液配比、載氣用量,得出這些工藝條件對收率的影響
2、,實驗表j盯j,儺化刺不經(jīng)過活化,原料液中含水分40%時可得到較好的轉(zhuǎn)化率和收率,反應(yīng)渝度380"(2,最高收率可達68%。并對這種催化劑進行了穩(wěn)定性實驗。接著以2一甲基吡嗪為原料,進行氣相氨氧化催化合成2一氰基吡嗪的實驗。分別用自制的三種催化劑進行了工藝研究。f其中Mo、PpⅨY型催化劑選擇性為‘\60%左右,收率可達40%以上,最合適的工藝條件是反應(yīng)溫度370"C,2一甲基璉匕嗪:氨氣:氧氣=i:2.5~3:6(摩爾比)。Sbz03一V205一TiOJSi02型催化剎。反應(yīng)溫度380"(2,2一甲基吡嗪:氨氣:氧氣=l:3~
3、6:8.5(摩爾比),選擇性在70%以上,收率可達55%以上,并進行了催化劑穩(wěn)定性實驗,證明該催化劑、~具有較好的穩(wěn)定性。J7關(guān)鍵詞:2一氰基吡嗪:2一甲基吡嗪:乙二胺:l,2一丙二醇:氨氧化:合1吣ABSTRACTTheusesofpyrazinederivativesinpharmaceuticalproducts.a(chǎn)griculturalchemicalsandspiceswereintroducedinthisthesis.Theresearchsituation,marketforegroundandresearchp
4、urposeofthegoalproductcyanopyrazinewerediscussed.Wealsosummarizedthemethodsofsythesisofcyanopyrazineand2-methylpylazine.First、ethylenediamineand1,2-dihydroxypropanewerechosenasrawmaterialstOprepare2-methylpylazinewiththemethodofcatalyticaction.ThecatalystWasKB-207mad
5、ebySichuanLianya.whichcompoundsCuO41.26%,ZnO41.79%,A12037.75%.ThereactionWasprecededinfixedbedcatalyticreactor.Theeffectsoftemperature,ratiooffeeds,thecartiergas’suselevelontheyieldwerestudied.Theexpedmentsshowed,whenthetemperatureWasabout380"(2,catalystWasnotactivat
6、ed,40%waterWasusedinthefeedfluid.thehighrateofconversionandyieldcanbeget.Thehighestyieldis68%.ThenammoxidationcatalyticsynthesisofcyanopyrazineWasstudiedwiththelawmaterial2-methylpyrazine.WestudiedtheprocessconditionswitllUSeofthreekindsofcatalystsmadebyourselves.The
7、yieldCangetmorethan40%whenusethecatalystMoxPy0:XY.Thebestprocessconditionistemperature370"(2,2-methylpyrazine:ammonia:oxygen=1:2.5-3:6fmoleratio).WhenSin03一V205一Ti02/Si02catalystWasused.theyieldcanbe55%,theselectivityismorethan70%.WhenthetemperatureWas380℃,2-methylpy
8、lazine:ammonia:oxygen=1:3~6:8.5(moleratio).Theexperimentsonstabilityofthecatalystwerealsodoneandtheresultshowsthatthiscatalystissta