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作 者:许浩然[1,2] 王海洋 王广兴[1,2] 金丹 王艳慧[1] 王静 XV Hao-ran;WANG Hai-yang;WANG Guang-xing;JIN Dan;WANG Yan-hui;WANG Jing(Sinosteel Anshan Research Institute of Thermo-energy Co.,Ltd.,Anshan Liaoning 10041,China;National and Local Joint Engineering Research Center of Coal tar New Material Preparation Technology,Anshan Liaoning10041,China)
机构地区:[1]中钢集团鞍山热能研究院有限公司,辽宁鞍山10041 [2]煤焦油系新型材料制备技术国家地方联合工程研究中心,辽宁鞍山10041
出 处:《当代化工》2022年第12期2874-2877,共4页Contemporary Chemical Industry
基 金:辽宁省“兴辽英才计划”项目(项目编号:XLYC2008003)。
摘 要:以咔唑和硫酸二乙酯为原料,利用超声波反应生成储氢N-乙基咔唑,反应液经过进一步处理得到纯品N-乙基咔唑。考察了反应用溶剂、反应温度及反应时间对N-乙基咔唑收率的影响。结果表明:合成产物的最佳溶剂是丙酮,最佳反应温度为40℃,超声波功率100 W,辐照频率40 kHz,最佳反应时间为1 min。产物经FTIR、^(1)HNMR进行结构表征。N-乙基咔唑的液相色谱纯度>99.5%,气相色谱纯度>99.5%,熔点68℃,总产率99%,合成产物可作为储氢材料使用。Using carbazole and diethyl sulfate as raw materials,hydrogen storage N-ethyl carbazole was prepared by ultrasonic reaction,and pure N-ethyl carbazole was obtained by further treatment of the reaction solution.The effects of solvent,reaction temperature and reaction time on the yield of N-ethyl carbazole were investigated.The results showed that the best solvent was acetone,the best reaction temperature was 40℃,ultrasonic power was 100 W,irradiation frequency was 40 kHz,and the best reaction time was 1 min.The structure of the product was characterized by FTIR and ^(1)H NMR.The liquid chromatographic purity of N-ethyl carbazole was>99.5%,the gas chromatographic purity was>99.5%,the melting point was 68℃,the total yield was 99%,and the synthesized product could be used as hydrogen storage material.
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