Micro-continuous flow technology for producing tonalide

Abstract

The invention discloses a micro-continuous flow technology for producing tonalide. The technology taking 1,1,3,4,4,6-hexamethyltetrahydronaphthalene (HMT) and acetyl chloride as raw materials, anhydrous aluminum chloride as a catalyst and dichloroethane and other organic matters as a solvent comprises the following steps: mixing the anhydrous aluminum chloride, the solvent and acetyl chloride under a low-temperature condition to obtain a catalyst phase; mixing and dissolving the raw material HMT with the solvent to obtain a raw material phase; respectively pre-cooling the raw material phase and the catalyst phase, and introducing the pre-cooled raw material phase and catalyst phase into a micro-channel reactor, and performing a reaction; and finally, introducing the obtained reaction product into a microstructure mixing module, quenching and layering the obtained reaction product, and then carrying out extraction, rotary evaporation, recrystallization and drying to obtain the tonalide.The micro-continuous flow technology has the advantages of short retention time, continuousness in operation, increase of the production efficiency of the product, improvement of the production safety and the product yield by timely removing heat in the reaction process, and reduction of the risk of the quenching process by timely removing heat in the quenching process.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a micro-continuous flow technology for producing musk. Background technique [0002] In view of the limited sources of natural musk and the high price, which is far from enough for people's demand for musk, it is urgent to develop synthetic musk with musk aroma to meet market demand, wherein musk (7-acetyl-1,1,3,4,4, 6-hexamethyl-1,2,3,4-tetrahydronaphthalene) is one of them. It belongs to the bicyclic tetralin type musk, with a strong powdery fragrance, excellent fragrance quality, elegant fragrance, and long-lasting fragrance, giving people a very comfortable and pleasant feeling. The product has strong diffusing power and good coordination. It is stable in the medium, not easy to change color, and has strong adhesion to fibers. It is suitable for high-end cosmetics such as soaps and face powders, as well as detergents and fabric softeners. It ...

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Problems solved by technology

[0005] In the disclosed methods of the above patents, the two-step synthesis reaction of musk is a Friedel-Crafts reaction carried out under low temperature conditions, and the heat release is very large. In order to control the reaction temperature, the reaction is usually carried out in a tank reactor. The way of adding is carried out, and the efficiency is very low; after the reaction, the reaction liquid needs to be quenched quickly with ice brine, and the quenching process involves a strong exothermic reaction between anhydrous aluminum trichloride and water. In order to control the quenching temperature, The quenching process usually requires a large amount of ice brine, and the operation also needs to be carried out slowly, and the efficiency is also very low

Therefore, the production process has problems such as small production scale, high operation cost, long operation time, and high risk, which does not meet the current requirements of the chemical industry for environmental protection and safety.

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