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A kind of circulation micro-reaction method of m-methyl anisole and used reaction device

A technology for m-methyl anisole and methyl anisole, which is applied in the field of chemical synthesis, can solve the problems of decreased utilization rate of dimethyl sulfate, strong alkalinity, etc., so as to improve the conversion rate of raw materials, inhibit alkaline decomposition, The effect of reducing the energy consumption of the reaction

Active Publication Date: 2022-04-22
SHANDONG DOCRIS CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of circulation micro-reaction method of m-methyl anisole and used reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Measure m-cresol and dimethyl sulfate according to the reaction molar ratio of 1:1.05. After being mixed by a micro-mixer, they are introduced into the reaction kettle. The reaction kettle is turned on and stirred for 2 minutes, and mixed evenly to form a circulating solution.

[0042] (2) After measuring according to the reaction molar ratio of m-cresol and sodium hydroxide as 1:1.08, the sodium hydroxide solution is introduced into the reaction kettle through the micro-mixer at a flow rate of 15ml / min, and the circulating solution is externally circulated The pipeline circulates through the micro-mixer, and enters the reaction kettle after being fully mixed with the sodium hydroxide solution in the micro-mixer; the circulating solution flows through the micro-mixer through the external circulation pipeline. The ratio of the circulating flow rate to the flow rate of the sodium hydroxide solution flowing through the micro-mixer is 6:1; the mixing temperature of the m...

Embodiment 2

[0045] (1) Measure m-cresol and dimethyl sulfate according to the reaction molar ratio of 1:1.1, mix them with a micro-mixer, and introduce them into the reaction kettle. Turn on the reaction kettle and stir for 3 minutes, and mix evenly to form a circulating solution.

[0046] (2) After measuring according to the reaction molar ratio of m-cresol and sodium hydroxide as 1:1.2, the sodium hydroxide solution is introduced into the reaction kettle through the micro-mixer at a flow rate of 10ml / min, and the circulating solution is externally circulated The pipeline circulates through the micro-mixer, and enters the reaction kettle after being fully mixed with the sodium hydroxide solution in the micro-mixer; the circulating solution flows through the micro-mixer through the external circulation pipeline. The ratio of the circulating flow rate to the flow rate of the sodium hydroxide solution flowing through the micro-mixer is 10:1; the mixing temperature of the micro-mixer and the ...

Embodiment 3

[0049] (1) Measure m-cresol and dimethyl sulfate according to the reaction molar ratio of 1:1.02. After being mixed by a micro-mixer, they are introduced into the reaction kettle. The reaction kettle is turned on and stirred for 1 minute, and mixed evenly to form a circulating solution.

[0050] (2) After measuring according to the reaction molar ratio of m-cresol and sodium hydroxide as 1:1.05, the sodium hydroxide solution is introduced into the reaction kettle through the micro-mixer at a flow rate of 15ml / min, and the circulating solution is externally circulated The pipeline circulates through the micro-mixer, and enters the reaction kettle after being fully mixed with the sodium hydroxide solution in the micro-mixer; the circulating solution flows through the micro-mixer through the external circulation pipeline. The ratio of the circulating flow rate to the flow rate of the sodium hydroxide solution flowing through the micro-mixer is 15:1; the mixing temperature of the m...

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Abstract

The invention discloses a circulating micro-reaction method of m-methylanisole and a reaction device used therefor, comprising the following steps: (1) Measuring m-cresol and dimethyl sulfate respectively according to the reaction molar ratio and then micro-mixing After being mixed with the container, it is introduced into the reaction kettle, and stirred evenly to form a circulating solution. (2) Quantitative sodium hydroxide solution is introduced into the reaction kettle through the micro-mixer according to a certain flow rate, and the circulating solution is circulated through the micro-mixer through the external circulation pipeline at the same time, and enters the reaction kettle after being fully mixed; (3) Sodium hydroxide After the solution is added, close the external circulation, maintain the temperature of the reactor and stir for 5 to 30 minutes, divide the reaction solution into two phases of oil and water, and extract the m-methylanisole product. The present invention adopts the form of circulation reaction, increases the contact area between sodium hydroxide and m-cresol, effectively reduces the concentration of sodium hydroxide in the reaction system, thereby inhibits the alkaline decomposition of dimethyl sulfate, and improves the reaction rate .

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis technology and device of m-methylanisole. Background technique [0002] M-methylanisole 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, methyl halide method, dimethyl carbonate method, etc. Among them, halogenated (chlorine, bromine, iodide) methane is a classic alkylation reagent. Although it has high reactivity, its boiling point is generally low, the operating conditions for synthesis are relatively harsh, and the price is expensive. As a new type of methylation reagent, the dimethyl carbonate meth...

Claims

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Application Information

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Patent Type & Authority Patents(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