New process for synthesis of musk ketone by microchannel reactor

Abstract

The invention discloses a new process for synthesis of musk ketone by a microchannel reactor. The process includes the steps of: S1. preparing an auxiliary catalyst; S2. mixing the auxiliary catalystwith a sulfuric acid solution to prepare a composite catalyst, mixing dichloroethane with acetic anhydride to prepare a mixed solvent, mixing the mixed solvent with 2, 6-dimethyl-4-tert-butylacetophenone evenly to obtain a material A, preheating the composite catalyst, a nitric acid solution and the material A respectively, and then conducting mixing; S3. carrying out mixing reaction, and drainingthe reaction liquid at the end of the reaction; and S4. quenching the reaction liquid by a quenching module to obtain musk ketone. The process provided by the invention employs a continuous microchannel reactor to synthesize musk ketone, and has the advantages of short reaction time, low reaction temperature, convenient operation, and high yield and output. The process thoroughly eliminates the danger of nitration reaction explosion in traditional intermittent kettle type reaction, achieves high yield continuous production of musk ketone, also the process produces little waste acid, and reduces the pressure of later sewage treatment.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a new process for synthesizing ketone musk by using a microchannel reactor. Background technique [0002] At present, there are three types of musk fragrances produced and used. Nitromusk accounts for about 50%, polycyclic musk accounts for 45%, and macrocyclic musk accounts for about 5%. Among them, nitromusk is the earliest synthetic musk fragrance developed. It has never been found in nature, and it is widely used in perfume essence, soap essence and cosmetic essence. Commonly used nitro musks are xylene musk and ketone musk. Ketone musk is 3,5-dinitro-2,6-dimethyl-4-tert-butylacetophenone (3,5-dinityl-2,6-dimethyl-4-tert-butylacetophenone), which is nitro A kind of musk, which has a soft musk aroma and is soluble in almost all spices. Due to the easy availability of raw materials and short synthesis route, this product is the cheapest synthetic musk. [0003] In ...

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the synthesis of ketone musk in the prior art mostly adopts batch reaction, the product yield is low, the energy consumption of separation and material consumption increase, and the pressure rises sharply in the reaction process, which is prone to spraying and burning , explosion problem, and proposed a new process for the synthesis of ketone musk using a microchannel reactor