三相相轉(zhuǎn)移催化法制備二氧化雙環(huán)戊二烯
發(fā)布時間:2018-06-11 15:01
本文選題:三相相轉(zhuǎn)移催化 + 二氧化雙環(huán)戊二烯 ; 參考:《應(yīng)用化學(xué)》2010年09期
【摘要】:以氯甲基化大孔聚苯乙烯-二乙烯基苯交聯(lián)樹脂(PS)接枝N-芐基-N,N-二甲基十二烷基季銨磷鎢雜多酸鹽為三相相轉(zhuǎn)移催化劑,質(zhì)量分?jǐn)?shù)為50%的工業(yè)雙氧水為氧化劑,制備了二氧化雙環(huán)戊二烯(DCPDDO)。采用FTIR和1HNMR對產(chǎn)物進(jìn)行表征。考察了溶劑和催化劑用量、物料摩爾比、反應(yīng)溫度和時間對環(huán)氧化反應(yīng)的影響。采用正交試驗法獲得的最佳反應(yīng)條件為(以0.05mol雙環(huán)戊二烯(DCPD)計):1,2-二氯乙烷18mL,催化劑2.25g,n(DCPD)∶n(H2O2)=1∶2.75,反應(yīng)溫度60℃,反應(yīng)時間12h。在此條件下,DCPDDO的收率可達(dá)89%以上,催化劑回收方便且重復(fù)使用7次未見活性明顯降低。
[Abstract]:N-benzyl-N-dimethyl-dodecylammonium phosphotungstophosphate heteropoly salt grafted with chloromethylated macroporous polystyrene-divinylbenzene crosslinked resin (PSPS) was used as a three-phase transfer catalyst and commercial hydrogen peroxide with a mass fraction of 50% was used as oxidant. Dicyclopentadiene oxide (DCPDDOA) was prepared. The products were characterized by FTIR and 1H NMR. The effects of the amount of solvent and catalyst, the molar ratio of materials, reaction temperature and time on the epoxidation reaction were investigated. The optimum reaction conditions obtained by orthogonal test were as follows: (0.05mol dicyclopentadiene dichloroethane 18ml), catalyst 2.25g DCPD: n H _ 2O _ 2H _ 2O _ 2H _ 2O _ 2: 2.75, reaction temperature 60 鈩,
本文編號:2005696
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