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Method for continuously producing 6-acetyl-1,1,2,4,4,7-hexamethyltetralin intermediate HMT by micro-reactor system

A micro-reactor, tunal musk technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, addition of unsaturated hydrocarbons and saturated hydrocarbons to produce hydrocarbons, etc., can solve the problem of large temperature rise in the quenching process. , easy to block the reactor, safety hazards and other problems, to avoid low product yield, avoid high risk, and strong competitiveness

Active Publication Date: 2020-09-01
FUZHOU UNIV
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  • 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

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  • Method for continuously producing 6-acetyl-1,1,2,4,4,7-hexamethyltetralin intermediate HMT by micro-reactor system
  • Method for continuously producing 6-acetyl-1,1,2,4,4,7-hexamethyltetralin intermediate HMT by micro-reactor 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...

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Abstract

The invention discloses a method for continuously producing a 6-acetyl-1,1,2,4,4,7-hexamethyltetralin intermediate HMT by a micro-reactor system, which comprises the following steps: uniformly mixinga catalyst with a weak polar solvent and a strong polar solvent to obtain a catalyst phase; then mixing 2, 3-dimethyl-1-butene, tert-butyl chloride and p-cymene to obtain a mixture which is used as araw material phase; pre-cooling the two strands of materials, introducing the pre-cooled materials and nitrogen into a cross-shaped micro-mixer for mixing, and enabling the mixture to enter a reactionsection for reaction; introducing the reaction product and an ice hydrochloric acid solution into a T-shaped micro-channel for quenching; and finally, carrying out layering, rectification, recrystallization and drying to obtain the 6-acetyl-1,1,2,4,4,7-hexamethyltetralin intermediate HMT. According to the method, by means of efficient heat transfer capacity of gas-liquid two-phase flow and gas-liquid-liquid three-phase flow in the micro-reactor, a large amount of heat generated in the reaction and quenching processes is rapidly removed, and the problems of low product yield and high risk caused by large temperature rise of the reaction are avoided. Besides, the adopted continuous process can greatly improve the productivity, effectively solves the defects in the existing HMT production process, and realizes 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

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Application Information

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Patent Type & Authority Applications(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