New process for synthesis of musk ketone by microchannel reactor

A micro-channel reactor, ketone musk technology, applied in the preparation of nitro compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. The problems of increased energy consumption and material consumption, and low product yield can achieve the effect of avoiding a large amount of use, reducing the amount of use, and shortening the reaction time.

Inactive Publication Date: 2019-02-01
濮阳市欧亚化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of new technology that adopts microchannel reactor to synthesize ketone musk that the present invention proposes comprises the following steps:

[0020] S1, preparation of auxiliary catalyst: take by weighing 15 parts by weight of chitosan, 10 parts by weight of zeolite powder, 2 parts by weight of tricyclohexylphosphine, 1 part by weight of palladium acetate, 3 parts by weight of phosphorus pentoxide, and a mass fraction of 20%. 5 parts by weight of acetic acid and 25 parts by weight of deionized water are used for subsequent use. Mix acetic acid and deionized water with a mass fraction of 20% evenly, heat up to 78° C., add chitosan, palladium acetate and phosphorus pentoxide by ultrasonic vibration and dissolve , heat preservation and stand still for 20 minutes to obtain a mixed solution, mix and grind tricyclohexylphosphine and zeolite powder to 170 mesh, then add to the mixed solution, condense and dry to obtain an auxiliary catalyst after ultrasonic vibration...

Embodiment 2

[0025] A kind of new technology that adopts microchannel reactor to synthesize ketone musk that the present invention proposes comprises the following steps:

[0026] S1, preparation of auxiliary catalyst: take by weight 20 parts by weight of chitosan, 14 parts by weight of zeolite powder, 3.5 parts by weight of tricyclohexylphosphine, 2 parts by weight of palladium acetate, 5 parts by weight of phosphorus pentoxide, and a mass fraction of 20%. 8 parts by weight of acetic acid and 35 parts by weight of deionized water are used for subsequent use. Mix 20% acetic acid and deionized water evenly, heat up to 88° C., add chitosan, palladium acetate and phosphorus pentoxide by ultrasonic vibration for dissolution , heat preservation and stand still for 30 minutes to obtain a mixed solution, mix and grind tricyclohexylphosphine and zeolite powder to 210 mesh, then add to the mixed solution, condense and dry to obtain an auxiliary catalyst after ultrasonic oscillation;

[0027] S2, by...

Embodiment 3

[0031] A kind of new technology that adopts microchannel reactor to synthesize ketone musk that the present invention proposes comprises the following steps:

[0032] S1, preparation of auxiliary catalyst: take by weighing 25 parts by weight of chitosan, 18 parts by weight of zeolite powder, 5 parts by weight of tricyclohexylphosphine, 3 parts by weight of palladium acetate, 8 parts by weight of phosphorus pentoxide, and a mass fraction of 20%. 12 parts by weight of acetic acid and 45 parts by weight of deionized water are used for subsequent use. Mix acetic acid and deionized water with a mass fraction of 20% evenly, heat up to 98° C., add chitosan, palladium acetate and phosphorus pentoxide by ultrasonic vibration and dissolve , heat preservation and stand still for 40 minutes to obtain a mixed solution, mix and grind tricyclohexylphosphine and zeolite powder to 250 meshes, then add to the mixed solution, condense and dry to obtain an auxiliary catalyst after ultrasonic vibra...

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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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/45C07C201/08B01J31/22
CPCB01J31/2226C07C201/08C07C205/45
Inventor 刘国朋邹宗鹏郜时国江秀全王福田路翠翠
Owner 濮阳市欧亚化工科技有限公司
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