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Loop micro-reaction method of m-methyl anisole and reaction device used in loop micro-reaction method

A technology for m-methyl anisole and methyl anisole, applied in the field of chemical synthesis, can solve the problems of decreased utilization rate of dimethyl sulfate, strong alkalinity, etc. The effect of reducing the energy consumption of the reaction

Active Publication Date: 2020-04-28
SHANDONG DOCRIS CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the former, the pH of the reaction system is high and the alkalinity is strong, which easily causes the alkaline hydrolysis of dimethyl sulfate, so that the utilization rate of dimethyl sulfate decreases

Method used

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  • Loop micro-reaction method of m-methyl anisole and reaction device used in loop micro-reaction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) m-cresol and dimethyl sulfate according to the reaction molar ratio of 1: 1.05, respectively measure and then introduce into the reactor after mixing by the micro-mixer, open the reactor and stir for 2 minutes, and mix uniformly to form a circulating solution.

[0042] (2) after being 1:1.08 metering according to the reaction mol ratio of m-cresol and sodium hydroxide, the sodium hydroxide solution is introduced into the reactor via the micro-mixer at the flow rate of 15ml / min, while the circulating solution is externally circulated The pipeline circulates through the micro-mixer, and enters the reactor after fully mixing with the sodium hydroxide solution in the micro-mixer; the circulating solution circulates through the external circulation pipeline through the micro-mixer. The ratio of the circulating flow rate to the flow rate of the sodium hydroxide solution flowing through the micro-mixer was 6:1; the mixing temperature of the micro-mixer and the temperature o...

Embodiment 2

[0045] (1) according to the reaction molar ratio of 1:1.1, m-cresol and dimethyl sulfate are respectively measured and introduced into the reaction kettle after being mixed by the micro-mixer, and the reaction kettle is opened and stirred for 3 minutes, and the mixture is uniformly formed to form a circulating solution.

[0046] (2) according to the reaction mol ratio of m-cresol and sodium hydroxide after being 1: 1.2 metering, the sodium hydroxide solution is introduced into the reactor by the flow rate of 10ml / min via the micro-mixer, while the circulating solution is externally circulated The pipeline circulates through the micro-mixer, and enters the reactor after fully mixing with the sodium hydroxide solution in the micro-mixer; the circulating solution circulates through the external circulation pipeline through the micro-mixer. The ratio of the circulating flow to the flow of the sodium hydroxide solution flowing through the micro-mixer was 10:1; the mixing temperature...

Embodiment 3

[0049] (1) m-cresol and dimethyl sulfate according to the reaction molar ratio of 1: 1.02, respectively measure and then introduce into the reactor after mixing by the micro-mixer, open the reactor and stir for 1 minute, and mix uniformly to form a circulating solution.

[0050] (2) after being 1:1.05 metering according to the reaction mol ratio of m-cresol and sodium hydroxide, the sodium hydroxide solution is introduced into the reactor via the micro-mixer at the flow rate of 15ml / min, while the circulating solution is externally circulated The pipeline circulates through the micro-mixer, and enters the reactor after fully mixing with the sodium hydroxide solution in the micro-mixer; the circulating solution circulates through the external circulation pipeline through the micro-mixer. The ratio of the circulating flow rate to the flow rate of the sodium hydroxide solution flowing through the micro-mixer was 15:1; the mixing temperature of the micro-mixer and the temperature o...

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Abstract

The invention discloses a loop micro-reaction method of m-methyl anisole and a reaction device used by the method, and the method comprises the following steps: (1) respectively metering m-cresol anddimethyl sulfate according to a reaction molar ratio, mixing by a micro-mixer, introducing into a reaction kettle, and uniformly stirring to form a circulating solution; (2) introducing a certain amount of sodium hydroxide solution into the reaction kettle through the micro-mixer according to a certain flow rate, simultaneously enabling the circulating solution to circularly flow through the micro-mixer through an external circulating pipeline, fully mixing and then entering the reaction kettle; and (3) after the sodium hydroxide solution is completely added, closing the external circulation,maintaining the temperature of the reaction kettle, carrying out a stirring reaction for 5-30 min, separating the reaction liquid into an oil phase and a water phase, and extracting to obtain the m-methyl anisole product. By adopting a loop reaction form, the contact area of sodium hydroxide and m-cresol is increased, and the concentration of sodium hydroxide in a reaction system is effectively reduced, so that alkaline decomposition of the dimethyl sulfate is inhibited, and the reaction rate is increased.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis technology and a device for m-methyl anisole. Background technique [0002] M-methyl anisole is an intermediate in organic synthesis, which can be used to synthesize medicines and pesticides. It is also an important raw material for pressure-sensitive and heat-sensitive dyes, and is widely used in the synthesis of fine chemicals. As a kind of oxyalkylation reaction of phenolic hydroxyl group, it can be obtained by reacting it with corresponding alkylating reagents, such as dimethyl sulfate method, halogenated methane method, dimethyl carbonate method, etc. Among them, halogen (chlorine, bromine, iodine) methane is used as a classic alkylating reagent. Although it has high reactivity, its boiling point is generally low, and the synthetic operating conditions are harsh and expensive. As a new type of methylation reagent, the dimethyl carbonate method has the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/205B01J19/00
CPCC07C41/16B01J19/0093C07C43/205
Inventor 王德强骆广生王凯卢凤阳类成存宋森鹏张鹏
Owner SHANDONG DOCRIS CHEM