|
|
|
| Research on methyl esterification of gulonic acid in a microchannel reactor |
| An Weihong, Lu Xiaoming |
| CSPC Weisheng Pharmaceutical(Shijiazhuang)Corporation Ltd., Shijiazhuang 050035, China |
|
|
|
|
Abstract In order to find an efficient synthesis process of methyl gulongate, promote the vitamin C raw material production industry to achieve energy conservation and green development. In this paper,methyl 2-keto-L-gulonate was synthesized in a microchannel reactor using 2-keto-L-gulonic acid and methanol as raw materials and concentrated sulfuric acid as catalyst. The effects of material ratio, catalyst dosage, reaction temperature and residence time on product content and conversion rate were investigated, and the technological parameters were optimized. The results show that when the reaction temperature is 85℃, the amount of concentrated sulfuric acid as catalyst can be reduced to 0.2%, and the reaction time can be shortened to 90 minutes;Compared with the traditional kettle synthesis process, the new process can reduce the amount of catalyst, eliminate the reaction amplification effect and temperature fluctuation, shorten the reaction time, and improve the safety of the process.
|
|
|
|
|
|
| [ 1 ] FANELLI F, PARISI G, DEGENNARO L, et al. Contribution of microreactor technology and flow chemistry to the development of green and sustainable synthesis [ J ]. Beilstein Journal of Organic Chemistry, 2017, 13( 1 ): 520 - 542.
[ 2 ] 王 磊,李 涛,张红艳. 强酸性阳离子交换树脂替代浓硫酸用于古龙酸甲酯化[ J ]. 世界饲料杂,2006 , ( 9 ):16 - 18.
[ 3 ] 李春艳,夏海平,蓝伟光. 维生素 C生产工艺进展 [ J ]. 中国医药工业杂志,2001,32( 1 ):38 - 41.
[ 4 ] 李 斌. 微反应器技术在精细化工中的应用[ J ]. 精细化工,2006,23( 1 ):1 - 7.
[ 5 ] 骆广生,王 凯,吕阳成,等. 微反应器最新研究进展[ J ]. 现代化工,2009,5:27 - 30.
[ 6 ] 何 伟,方 正,陈克涛,等. 微反应器在合成化学中的应用[ J ]. 应用化学,2013,30( 12 ):1 376 - 1 381.
[ 7 ] 张 跃,张 菁,辜顺林,等. 微通道中硝基胍的连续流合成[ J ]. 精细化工,2016,33( 8 ):946 - 950.
[ 8 ] Roberge D M, Ducry L, Bieler N, et al. Micro-reactor technology: a revolution for the fine chemical and pharmaceutical industries [ J ]. Chem Eng Technology, 2005, 28( 3 ): 318 - 323.
[ 9 ] Pohar A, Plazl I. Laminar to Turbulent Transition and Heat Trans-
fer in a Microreactor: Mathematical Modeling and Experiments[ J ]. Ind Eng Chem Res, 2008, 47( 19 ): 7 447 - 7 455.
[ 10 ] 吴 迪,高朋召. 微反应器技术及其研究进展[ J ]. 中国陶瓷工业,2018,25( 8 ):19 - 26. |
|
|
|