Method for synthesis of 2,2,4-trimethyl-1,2-dihydroquinoline and polymer thereof by utilizing microchannel reactors

Abstract

The invention relates to a method for synthesis of 2,2,4-trimethyl-1,2-dihydroquinoline and a polymer thereof by high-throughput microchannel reactors. A mixture of acetone and aniline hydrochloride is used as a starting reaction raw material and is injected into a microchannel reactor system for reaction, wherein the microchannel reactor system is composed of 1-10 pieces of microchannel reactors which are connected together in series and can be used for continuous flowing, the single-piece reactors are connected together in series by microchannels having the shape similar to a heart shape, and the liquid holdup amount is 8-10 ml; and a continuous flowing reaction is carried out. Through a heat carrier circulation system, the reaction temperature is set to 90-120 DEG C, the pressure is set to 0-10 bar, and the reaction standing time is set to 20-200 s; the obtained solution is cooled by a condenser and is collected, unreacted acetone is removed by distillation, and the target product is obtained. The preparation method provided by the invention has the advantages of continuous reaction performing, short required reaction time, no amplification effect, and strong versatility, does not require to remove generated water during the reaction process, and can be applied to various liquid-liquid, gas-liquid and other chemical reactions.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for polycondensation of ketones and amines using a high-throughput microchannel reactor, especially for the synthesis of 2,2,4-trimethyl-1, In the synthesis of 2-dihydroquinoline compounds. Background technique [0002] 2,2,4-Trimethyl-1,2-dihydroquinoline and its polymers are mainly used to prepare quinoline rubber antioxidants, including rubber antioxidant RD and antioxidant FR. The synthesis method is in the acid In the presence of a catalyst, aniline and acetone are prepared by polycondensation reaction. The reaction generally adopts a gap reactor. In some reaction processes, the water generated in the reaction must be taken out by solvents to ensure that the reaction can continue to proceed forward. [0003] At present, the production method of dihydroquinoline compounds at home and abroad is mainly to carry out polycondensation reaction of aniline and acet...

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that after the catalyst p-toluenesulfonic acid, hydrochloric acid and zinc chloride are consumed, they cannot be regenerated and recycled, there are many waste liquids, severe corrosion, and high toxicity of toluene

This method avoids the corrosion of the equipment by the liquid acid catalyst, and can be connected for reaction. The disadvantage is that the required reaction equipment is very large and the reaction time is long.

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