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1、天津大學(xué)碩士學(xué)位論文酮連氮水解制肼的研究姓名:楊元生申請(qǐng)學(xué)位級(jí)別:碩士專業(yè):化學(xué)工藝指導(dǎo)教師:米鎮(zhèn)濤2000.1.1摘要本文制備并提純了丙酮連氮和丁酮連氮,以其為原料,研究了酮連氮常壓水解精餾和丁酮連氮水解反應(yīng)動(dòng)力學(xué),測(cè)得了丙酮連氮.丙酮、丁酮連氮.丁酮二元體系在常壓下的汽液平衡數(shù)據(jù),提出了它們的計(jì)算方法。影響酮連氮水解收率的因素之一是原料配比,實(shí)驗(yàn)給出了最佳摩爾配比:丙酮連氮:水=1:7,此時(shí)非催化水解收率可達(dá)51%。在選擇的幾種催化劑中,弱酸性陽(yáng)離子樹脂對(duì)于酮連氮的水解具有較商的活性,D114催化活性最高,顯著的提高了收率。催化劑的裝填位置對(duì)肼的收率有顯著影響,催化劑的合適裝填位置為塔的中
2、部。建立了丙酮連氮.肼.水體系的分析方法:采用丙酮作為掩蔽劑掩蔽肼,把分析丙酮連氮.肼.水體系轉(zhuǎn)化為分析丙酮連氮-丙酮.水體系,采用氣相色譜分析,避免了分析強(qiáng)極性的肼帶來(lái)的困難。研究了非催化和催化條件下丁酮連氨水解反應(yīng)動(dòng)力學(xué),得到了宏觀動(dòng)力學(xué)方娟下:丁酮連氮非催化水解反應(yīng)動(dòng)力學(xué)方程為:r:一孥:5.7156P一—20『90.51c』00977G叭066—4.5364e一面122.5—7Cc0’1mCD01143dt丁酮連氮催化水解動(dòng)力學(xué)方程為:r:一孥:3.0070P一—78礦8.12巴0‘1574G。_2060—4.3677P一百53.25cc。.0755cD乩1149dt測(cè)定了常壓下丙酮連
3、氮.丙酮、丁酮連氮一丁酮二元物系的恒壓汽液平衡數(shù)據(jù),并對(duì)其進(jìn)行了關(guān)聯(lián),得出了Wilson方程的參數(shù):丙酮連氮-丙酮物系:A2。=·O.3692;丁酮連氮.丁酮物系:A2。=-O.6083:A12=1.0366)——廠—一?A1220.6164/關(guān)鍵詞:肼丁酮連氮丙酮連氮水解精餾汽液平衡天津大學(xué)碩士學(xué)位論文AbstractPreparinghydrazinebyreactiondistillation,kineticsabouthydrolysisprocessofmethylethylAzine,theisobaricVapor-Liquid—Equilibriumofacetoneazine
4、-acetoneandmethylethylazine—butanonebinarysystemwerestudiedusingmaterialself-preparedinthiswork.Theratiooffeedisoneoffactorswhichinfluencedtheyieldofhydrazinesignificantly,theoptimumratioofazineandwaterwasl:7,andtheyieldofhydrazineismore也an5l%.Theweakacidcationicresincatalystshowedhighactivityforpre
5、paringhydrazine,andD114wasthemostactivecatalystinthem.Theplaceofcatalystloadedinfluencetheyieldsignificantly,theoptimumplaceofloadingthecatalystwasinthemiddleofdistillationcolun'm.Thesystemofacetoneazine·hydrazine-watercanbetransformedtoacetoneazine—acetone-waterbyacetonetoconcealhydrazine,andthesys
6、temofacetoneazine—acetone-watercanbeanalyzedbyGCeasily.Kineticreactionofhydrolysisprocessofmethylethylazinewasstudiedandequationsofkineticswithoutcatalystandwithcatalystwereasfollows.,:一孥:5.71569一—20頁(yè)90廠.51巳00977G0’1066—4.5364P一]122『.57Cc0’1126CD0‘1143口f,=一dC_,叢.A=3.0070e一—曠巳仉1州G。。206。一4.3677e一百cc00
7、755%m1149alDataoftheisobaricVapor-Liquid-Equilibriumofacetoneazine—-acetoneandmethylethylazine-butanonebinarysystemwereobtained,andtheparametersofWilsonEquationobtainedbyregressionWel'easfollows.a(chǎn)ceto