A circular microreaction method to the safe and efficient synthesis of 3-methylpyridine-N-oxide

3-Methylpyridine-N-oxide is an essential intermediate in the preparation of 2-chloro-5-methylpyridine,which can be used to synthesize nicotine insecticides such as imidacloprid and acetamiprid.The traditional method of production of 3-methylpyridine-N-oxide is catalytic oxidation of 3-methylpyridine in semi-batch reactors.Due to strong exothermic reaction and explosive property of 3-methylpyridine,the reaction efficiency and safety is low using batch technology.Therefore,the development of a safer and efficient 3-methylpyridine-N-oxide production process is very necessary in industrial production.In this paper,microreaction systems were introduced into the preparation of 3-methylpyridine-N-oxide.The comparison of three different methods(traditional semibatch method,co-current microreaction method,and circular microreaction method)showed that the circular microreaction method was the most applicable,with relative higher product yield(~90%),less side reaction and better reaction control.

Efficient extraction and stripping of Nd(Ⅲ),Eu(Ⅲ) and Er(Ⅲ) by membrane dispersion micro-extractors

The extraction of low concentration rare earth elements at high phase ratio was investigated. The traditional extraction set-up, such as mixer-settler, have drawbacks of easy emulsification, difficult separation and low efficiency if operated at the above condition. Membrane dispersion micro-extractor,owing to its well-dispersed, high surface-to-volume ratio and fast mass transfer rate, was employed in our work. Nd（Ⅲ）,Eu（Ⅲ）,Er（Ⅲ） were chosen to represent light, medium,heavy rare earth elements（REEs）. The extraction process of REEs with 2-ethylhexyl phosphoric acid-2-ethylhexyl ester（P507） was investigated by membrane dispersion micro-extractors. Firstly, the extraction equilibrium of these three elements was explored in the stirred conical flasks, and it is indicated that the extraction efficiencies can be 0.95, 0.97 and 0.98, respectively within 40 min at phase ratio of 100：1. Then the effects of operational conditions such as the residence time, organic and aqueous flow rates on extraction efficiency were also explored in micro-extractors. The results indicate that the efficiency decreases and then increases if increasing aqueous phase flow rate, residence time and droplets＇ diameter are the key factors of this process. Increasing the phase ratio reduces the extraction efficiency significantly. When the REEs solution has an initial pH of 4.00, the flow rates of continuous and dispersed phase are 40 and 1.6 mL/min,respectively, and 90 mg/L Nd（Ⅲ）, Eu（Ⅲ） and Er（Ⅲ） is extracted by 1 mol/L P507 at the out-let length of8 m. The extraction efficiencies are 0.978,0.983 and 0.991, respectively. Finally the stripping process was also studied with the micro-extractor. The stripping efficiencies of Nd（Ⅲ）, Eu（Ⅲ） and Er（Ⅲ） can reach0.99, 0.96 and 0.91, respectively when the out-let length is 8 m and the concentration of hydrochloric acid is 1 mol/L. The developed approach offers a novel and simple strategy on the fast extraction and enrichment of low concentration rare earth elements from waste water.