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机构地区:[1]江西省精细化工重点实验室江西师范大学,江西南昌330027
出 处:《石油化工》2010年第1期28-31,共4页Petrochemical Technology
基 金:国家自然科学基金资助项目(20566004);国家科技攻关计划资助项目(2001BA323C)
摘 要:以铌酸为主催化剂、三(3,6-二氧杂庚基)胺(TDA-1)为助催化剂,以环戊烯和水为原料,通过水合加成反应合成了环戊醇;考察了原料配比、反应温度、反应时间、催化剂用量、助催化剂种类等因素对环戊醇收率的影响;并用红外光谱表征了产物的结构。实验结果表明,与三乙胺、四丁基溴化铵和四丁基硫酸氢铵相比,TDA-1的助催化效果最好;铌酸的催化活性明显高于DNW-1阳离子交换树脂、固体酸、沸石和硫酸。该反应的最佳工艺条件为:环戊烯用量1.0mol,n(水)∶n(环戊烯)=4.0,铌酸用量4.0g,TDA-1用量0.8g,反应温度120℃,反应压力1.2MPa,反应时间4.0h。在此条件下,环戊醇的收率为68.1%,产品纯度为99.1%。Cyclopentanol was synthesized from cyclopentene and water through hydration reaction with niobic acid as catalyst and tris ( dioxa-3,6-heptyl ) amine ( TDA-1 ) as cocatalyst. Effects of n(H20):n(cyclopentene), reaction temperature, reaction time, catalyst dosage and cocatalyst type on cyclopentanol yield were investigated. The structure of the product was characterized by means of IR. Among four cocatalysts, namely triethylamine, tetrabutyl ammonium bromide, tetrabutyl ammonium bisulfate and TDA-1, TDA-1 was the best in catalytic performance. In catalytic activity niobic acid was significantly stronger than DNW-1 cation exchange resin, solid acid, zeolite and sulfuric acid. Under optimal reaction conditions: 1.0 mol cyclopentene, n (water) : n (cyclopentene) 4.0, niobic acid 4.0 g, TDA-1 0.8 g, reaction temperature 120 ℃, reaction pressure 1.2 MPa and reaction time 4.0 h, yield and purity of cyclopentanol were 68.6 % and 99.1%, respectively.
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