Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of method for the continuous production of musk intermediate HMT by microreactor system

A technology of microreactor and breathing musk, which is applied in the direction of chemical instruments and methods, chemical/physical/physicochemical reactors, addition of unsaturated hydrocarbons and saturated hydrocarbons, etc. The problem of large temperature rise and potential safety hazards during the extinguishing process is achieved, and the effect of high-efficiency heat transfer and avoiding large temperature rise is achieved.

Active Publication Date: 2021-09-28
FUZHOU UNIV
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The first two patents both adopt batch production process, which has two obvious disadvantages: (1) The exothermic heat of the reaction is violent and difficult to control, resulting in high temperature in the kettle, which is not conducive to improving selectivity; (2) The auxiliary operation time is long, resulting in Small scale of production
Although the third patent adopts a continuous process, there are still some problems: (1) The catalyst is easy to block the reactor when it is filled into the tubular reactor, resulting in poor fluidity; (2) Since the reactor is made of metal, the hydrogen chloride produced by the reaction The gas will seriously corrode it; (3) The temperature rise in the quenching process of the reaction is relatively large, and there are certain safety hazards

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
  • A kind of method for the continuous production of musk intermediate HMT by microreactor system
  • A kind of method for the continuous production of musk intermediate HMT by microreactor system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]In this embodiment, the dichloroethane (strong polar solvent) and cyclohexane (weak polar solvent) introduced into the catalyst phase are mixed with the 2,3-dimethyl-1-butene in the raw material phase. The molar ratio is 1.5:2:1; the molar ratio of the catalyst in the catalyst phase to the 2,3-dimethyl-1-butene in the raw material phase is 0.15:1. The molar ratio of 2,3-dimethyl-1-butene, cymene and tert-butyl chloride in the raw material phase is 1:2:1.1. The catalyst phase flow rate is 0.144~3.597ml / min; the raw material phase flow rate is 0.233~5.823ml / min; the residence time in the reaction section is 1~25min, and the reaction temperature is 15°C.

[0037] In the present embodiment, the nitrogen flow rate is within the range of 0.12 ~ 7.86ml / min, and the liquid phase is cut into several cylinders in the reaction section and the quenching section of the microreactor system; the flow rate of the glacial hydrochloric acid solution is at In the range of 0.38~9.50ml / min,...

Embodiment 2

[0044] The difference between embodiment 2 and example 1 is that catalyst consumption is different.

[0045] In this embodiment, the dichloroethane (strong polar solvent) and cyclohexane (weak polar solvent) introduced into the catalyst phase are mixed with the 2,3-dimethyl-1-butene in the raw material phase. The molar ratio is 1.5:2:1; the molar ratio of the catalyst in the catalyst phase to the 2,3-dimethyl-1-butene in the raw material phase is 0.17:1. The molar ratio of 2,3-dimethyl-1-butene, cymene and tert-butyl chloride in the raw material phase is 1:2:1.1. The catalyst phase flow rate is 0.144~3.597ml / min; the raw material phase flow rate is 0.233~5.823ml / min; the residence time in the reaction section is 1~25min, and the reaction temperature is 15°C.

[0046] In the present embodiment, the nitrogen flow rate is within the range of 0.12 ~ 7.86ml / min, and the liquid phase is cut into several cylinders in the reaction section and the quenching section of the microreactor...

Embodiment 3

[0052] The difference between embodiment 3 and embodiment 1 is that the reaction temperature is different. The residence time in the reaction section is 1~25min, and the reaction temperature is 10°C.

[0053] In this embodiment, the dichloroethane (strong polar solvent) and cyclohexane (weak polar solvent) introduced into the catalyst phase are mixed with the 2,3-dimethyl-1-butene in the raw material phase. The molar ratio is 1.5:2:1; the molar ratio of the catalyst in the catalyst phase to the 2,3-dimethyl-1-butene in the raw material phase is 0.15:1. The molar ratio of 2,3-dimethyl-1-butene, cymene and tert-butyl chloride in the raw material phase is 1:2:1.1. The catalyst phase flow rate is 0.144~3.597ml / min; the raw material phase flow rate is 0.233~5.823ml / min; the residence time in the reaction section is 1~25min, and the reaction temperature is 10°C.

[0054] In the present embodiment, the nitrogen flow rate is within the range of 0.12 ~ 7.86ml / min, and the liquid phas...

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 method for continuously producing musk intermediate HMT by a microreactor system. Firstly, the catalyst is uniformly mixed with a weak polar solvent and a strong polar solvent as a catalyst phase; then 2,3-dimethyl ‑1‑butene, tert-butyl chloride and p-cymene are mixed as the raw material phase; the two materials are pre-cooled and mixed with nitrogen into a ten-type micro-mixer, and enter the reaction section for reaction; and then mixed with ice hydrochloric acid solution Pass through T-shaped microchannel for quenching; finally, after layering, rectification, recrystallization and drying, HMT, an intermediate of Tuna musk, is obtained. With the help of the efficient heat transfer capacity of the gas-liquid two-phase flow and the gas-liquid-liquid three-phase flow in the microreactor, the method quickly removes a large amount of heat generated during the reaction and quenching process, avoiding the low product yield and high temperature caused by the large temperature rise of the reaction. high-risk issues. In addition, the continuous process adopted can greatly increase production capacity, effectively solve the defects existing in the existing HMT production process, and realize green and safe production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a method for continuously producing HMT, an intermediate of Tuna musk, by a microreactor system. Background technique [0002] Tuna musk is a kind of synthetic musk, which belongs to bicyclic tetralin musk. It is safe to use, harmless to human skin, has excellent fragrance quality, long-lasting fragrance, strong diffusing power, good coordination, stable in acid-base medium, strong adhesion to fibers, and has a wide range of uses. This product is an internationally recognized ideal fragrance, and its sales volume ranks first among synthetic musks. The domestic supply is currently in short supply. The synthesis of Tuna musk is mainly divided into two steps: one is to synthesize the intermediate HMT, and the other is to synthesize Tuna musk from the intermediate HMT. Wherein, the height of musk productive rate mainly depends on the productive rate...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/72C07C13/48B01J19/00B01J19/02
CPCB01J19/0093B01J19/02B01J2219/025C07C2/72C07C2527/126C07C2527/128C07C2527/138C07C2602/10C07C13/48
Inventor 王晓达汪世玮王清莲邱挺王红星叶长燊葛雪惠
Owner FUZHOU UNIV