Micro-continuous flow technology for producing tonalide

A technology of musk tona and micro-continuous flow, applied in chemical/physical/physical-chemical processes, organic chemistry, chemical/physical/physical-chemical reactors, etc., can solve the problems of long operation time, high risk and high operation cost , to achieve the effect of reducing raw material loss, easy operation and improving safety

Inactive Publication Date: 2020-04-03
FUZHOU UNIVERSITY
View PDF2 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Micro-continuous flow technology for producing tonalide
  • Micro-continuous flow technology for producing tonalide
  • Micro-continuous flow technology for producing tonalide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] combined with figure 2As shown, the processing equipment of the present embodiment comprises metering pump a1, metering pump b2 and metering pump c3, and described metering pump a1 links to each other with the first inlet of T-type passage mixer a401 in the microchannel reactor 4, and described metering pump b2 links to each other with the second inlet of the T-shaped channel mixer a401 in the microchannel reactor 4, and the third inlet of the T-shaped channel mixer a401 in the microchannel reactor 4 links to each other with the inlet of the reaction module 402, and the outlet of the reaction module 402 is connected with the microstructure The first inlet of the T-shaped channel mixer b in the mixer 5 is connected, the outlet of the metering pump c3 is connected with the second inlet of the T-shaped channel mixer b, and the third inlet of the T-shaped channel mixer b is connected with the quenching module 502 is connected to the inlet, and the outlet of the quenching m...

Embodiment 2

[0049] This embodiment is consistent with the operation steps of embodiment 1, only acetyl chloride, catalyst AlCl 3 And the molar ratio of dichloroethane was changed to 1:2:5. The conversion rate of HMT and the yield of products were analyzed by GC. In this example, the conversion rate of HMT was 99.5%, the yield of AHMT was 95.3%, and the purity was 98.5%.

Embodiment 3

[0053] This embodiment is consistent with the operation steps of embodiment 1, only acetyl chloride, catalyst AlCl 3 The molar ratio of dichloroethane and dichloroethane was changed to 1:0.5:7. The conversion rate of HMT and the yield of products were analyzed by GC. In this example, the conversion rate of HMT was 99.5%, the yield of AHMT was 93.6%, and the purity was 98.5%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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 ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C45/46C07C49/792B01J19/00
CPCB01J19/0093C07C45/46C07C2602/28C07C49/792
Inventor 王晓达汪世玮葛雪惠邱挺王红星王清莲陈锦溢黄智贤叶长燊李玲
Owner FUZHOU UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap