摘要
以Raney-Ni为催化剂在乙酸丁酯溶剂中,间歇催化2,3,5-三甲基苯醌(TMBQ)加氢合成2,3,5-三甲基氢醌(TMHQ)。通过正交实验考察了催化剂用量、溶剂用量、温度及压力等对反应的影响。结果表明,较优反应条件为:TMBQ初始浓度为0.1 g/mL,催化剂量为TMBQ的10%,氢气压力0.7～0.8 MPa,温度为100℃(转速800 r/min)。TMHQ加氢收率可达97.3%。溶剂通过水蒸气蒸馏回收,总收率93.1%。
An efficient and green process of catalytic hydrogenation of 2,3,5-trimethylbenzoquinone（TMBQ） to 2,3,5-trimethylhydroquinone（TMHQ） on Raney-Ni catalyst using the n-butyl acetate as solvent is described.Effect of temperature,catalyst loading,initial concentration of TMBQ and hydrogen pressure on reaction were investigated.Results showed that the optimal process conditions were as follows：0.1 g/mL initial concentration of TMBQ,10% catalyst loading,0.7～0.8 MPa hydrogen pressure,100 ℃ reaction temperature（800 r/min agitation）.The hydrogenation molar yield of TMHQ by HPLC analysis is 97.3%.The solvent could be recovered by steam distillation,while the isolated TMHQ overall molar yield reaches up to 93.1%.
出处
《应用化工》
CAS
CSCD
2013年第8期1363-1366,共4页
Applied Chemical Industry
基金
国家自然科学基金(21103121)
高等学校博士学科点专项科研基金(20110032120011)
