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Method for continuously producing methyl acetoacetate by using micro-channel reactor

A micro-channel reactor, methyl acetoacetate technology, applied in organic chemistry, ketene/polyketene preparation and other directions, can solve the problems of easy temperature out of control system, unsuitable for industrial production, long reaction time, etc., to avoid The effect of flying temperature phenomenon, short production cycle and stable reaction process

Inactive Publication Date: 2020-04-21
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the tank reactor used in this process does not realize continuous flow operation in a real sense, and does not solve the problem that the system is prone to soaring temperature and out of control during the reaction process, and the reaction time is long, so this process is not suitable for the trend of industrial production in the future

Method used

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  • Method for continuously producing methyl acetoacetate by using micro-channel reactor
  • Method for continuously producing methyl acetoacetate by using micro-channel reactor
  • Method for continuously producing methyl acetoacetate by using micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Device: continuous flow microchannel reaction device (3a+3a), refer to figure 2 Determine the connection mode of the microchannel reactor, the length of the microchannel is determined according to the flow rate and the reaction residence time, and the heat transfer medium is heat transfer oil.

[0029] (2) Preparation of methyl acetoacetate: adjust the microchannel reaction device to be a preheating zone, a reaction zone and a quenching zone according to the needs of the reaction process. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 30s, the preheating temperature and the reaction temperature are set to 70° C., and the reaction pressure is 5 bar. The mixture of substrate methanol and catalyst sulfuric acid is fed into preheating zone A of the device through metering pump 1, and diketene is fed into preheating zone B of the device through pump 2. After the two materials are ...

Embodiment 2

[0031] (1) Device: continuous flow microchannel reaction device (3a+3b), refer to figure 2 Determine the connection mode of the microchannel reactor, the length of the microchannel is determined according to the flow rate and the reaction residence time, and the heat transfer medium is heat transfer oil.

[0032](2) Preparation of methyl acetoacetate: adjust the microchannel reaction device to be a preheating zone, a reaction zone and a quenching zone according to the needs of the reaction process. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 60s, the preheating temperature and the reaction temperature are set to 80° C., and the reaction pressure is 10 bar. The mixture of substrate methanol and catalyst oxalic acid is fed into preheating zone A of the device through metering pump 1, and diketene is fed into preheating zone B of the device through pump 2. After the two streams of mater...

Embodiment 3

[0034] (1) Device: continuous flow microchannel reaction device (3a+3c), refer to figure 2 Determine the connection mode of the microchannel reactor, the length of the microchannel is determined according to the flow rate and the reaction residence time, and the heat transfer medium is heat transfer oil.

[0035] (2) Preparation of methyl acetoacetate: adjust the microchannel reaction device to be a preheating zone, a reaction zone and a quenching zone according to the needs of the reaction process. By adjusting the flow rate of the pump and the channel length of the microchannel, the residence time of the reaction is controlled to be 90s, the preheating temperature and the reaction temperature are set to 90° C., and the reaction pressure is 15 bar. The mixture of substrate methanol and catalyst citric acid is fed into preheating zone A of the device through metering pump 1, and diketene is fed into preheating zone B of the device through pump 2. After the two streams of mate...

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Abstract

The invention discloses a method for continuously producing methyl acetoacetate by using a micro-channel reactor, and belongs to the technical field of organic synthesis processes. Diketene and absolute methanol are used as raw materials, an acid or alkali is used as a catalyst, and the preparation process of methyl acetoacetate is continuously completed in a micro-channel reactor system. According to the method, after materials are fed into a micro-channel reactor through metering pumps, preheating, mixing, reacting and separation are performed to obtain a methyl acetoacetate product. In themethod, the temperature and the residence time during the reaction process can be strictly controlled, the reaction temperature can be accurately controlled so as to prevent temperature runaway, and the safety of the reaction apparatus can be improved; due to the strong mass transfer effect of the micro-channel reactor, the mass transfer effect among the raw materials in the reaction system is enhanced, and the reaction efficiency is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and specifically relates to a method for preparing methyl acetoacetate by esterification reaction using diketene as a raw material, more specifically, the continuous production of acetyl acetate by esterification reaction using diketene as a raw material in a microchannel reactor. Methyl acetate method. Background technique [0002] Methyl acetoacetate is an important intermediate of diazinon, which is widely used in the organic synthesis industry. It can also be used as a solvent for fiber resins, and to synthesize pharmaceuticals and pesticides. At present, the domestic production capacity is about 12,000 tons, and the actual production volume is about 5,500 tons. Its demand is rising day by day, and it is particularly urgent to increase its yield and reduce its raw material cost. [0003] CN103450017A discloses a method for preparing methyl acetoacetate, which is characte...

Claims

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Application Information

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IPC IPC(8): C07C67/46C07C69/72
CPCC07C67/46C07C69/72
Inventor 刘建武蒋晗严生虎张跃沈介发辜顺林马晓明陈代祥
Owner CHANGZHOU UNIV
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