Method for continuously producing m-diethylaminophenol through channelization

An ethylaminophenol and production room technology, which is applied in the field of pipeline continuous production of m-diethylaminophenol, can solve the problems of long reaction time, unsuitability for industrialization and the like, and achieves the effects of stable product quality, suppression of side reactions and good selectivity.

Active Publication Date: 2014-12-31
上海鸿源鑫创材料科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process uses relatively expensive bromoethane, and also uses sodium carbonate as an acid-binding agent. The reaction time is long and it is not suitable for industrialization.

Method used

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  • Method for continuously producing m-diethylaminophenol through channelization
  • Method for continuously producing m-diethylaminophenol through channelization
  • Method for continuously producing m-diethylaminophenol through channelization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A production device for pipelined continuous production of m-diethylaminophenol, its structure is as follows figure 1 As shown, it consists of a tubular reactor connected with other equipment. Tubular reactor 3 and raw material storage tank 1 are connected by metering pump 2, and the metering pump is used to transport the material from the raw material storage tank to the stainless steel coil pipe (tube length 20m, inner diameter 4mm, cross-sectional area about 0.13cm 2 , the volume is about 260mL) in the tubular reactor, the flow rate of the material can be controlled by a metering pump, and the tubular reactor is placed in a casing with a heating medium (for controlling the reaction temperature). The material enters the tubular reactor from the left side of the tubular reactor; the reaction mixture product flows out from the right side of the tubular reactor, and then flows into the storage tank 4 located in the cooling tank 5 to be cooled (cooling down to room temper...

Embodiment 2

[0030] A method for pipelined continuous production of m-diethylaminophenol, adopting the device of embodiment 1, taking m-aminophenol and ethyl chloride as raw materials, and carrying out the following steps successively:

[0031] (1) Preheat the tubular reactor 3 to 100°C, inject 260ml of ethanol (as a solvent) into the tubular reactor with the flow pump 2, so that the tubular reactor is filled with ethanol. Dissolve 16.4g (0.15mol) of m-aminophenol and 19.8g (0.31mol) of ethyl chloride in 200ml of ethanol to prepare about 225ml of material solution. The material solution is stored in raw material storage tank 1, and the temperature of the material solution is maintained at 10°C about. Use a flow pump to inject the material solution into the tubular reactor for reaction at a flow rate of 2ml / min;

[0032] The reaction temperature is 100°C, and the reaction time (that is, the residence time of the material in the tubular reactor) and the time for injecting the material solut...

Embodiment 3

[0038] A method for pipelined continuous production of m-diethylaminophenol, adopting the device of embodiment 1, taking m-aminophenol and ethyl chloride as raw materials, and carrying out the following steps successively:

[0039] (1) Preheat the tubular reactor to 80°C, inject 260ml of methanol (as a solvent) into the tubular reactor with a flow pump, so that the tubular reactor is filled with methanol. Dissolve 16.4g (0.15mol) of m-aminophenol and 25.6g (0.4mol) of ethyl chloride in 200ml of methanol to prepare about 230ml of material solution. The material solution is stored in the raw material storage tank, and the temperature of the material solution is maintained at about 10°C . Use a flow pump to inject the material solution into the tubular reactor for reaction at a flow rate of 2ml / min;

[0040] The reaction temperature is 80°C, and the reaction time (that is, the residence time of the materials in the tubular reactor) is about 115 minutes.

[0041] (2) Use the sto...

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Abstract

The invention belongs to the field of organic synthesis, and relates to a method for continuously producing m-diethylaminophenol through channelization. The method comprises the steps: (1) injecting a solvent into a pipe type reactor by a flow pump; dissolving the m-aminophenol and chloroethane into alcohol solvent according to the mole ratio of 1:(2-1.5) to prepare material solution; and injecting the material solution into the pipe type reactor by the flow pump, wherein the reaction temperature is 80-150 DEG C; (2) collecting reactive product flowing out of the pipe type reactor, removing the solvent and adding excessive alkaline for cleaning; and (3) extracting after the liquid is subjected to alkaline cleaning, taking water phase, adding acid for neutralizing to be neutral. The method is mild in reaction conditions, high in yield, good in selectivity, capable of effectively controlling the back-mixing and inhibiting the occurrence of side reaction, and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to a method for pipelined continuous production of m-diethylaminophenol. Background technique [0002] m-Diethylaminophenol, whose molecular formula is C 10 h 15 NO, its structural formula is as follows: [0003] [0004] m-Diethylaminophenol is an important intermediate used in dyes, medicines, cosmetics, etc., and is widely used in heat and pressure sensitive dyes. Among them, in the dye industry, it is an intermediate of dyes such as rhodamine, acid pink, and basic rhodamine. [0005] Currently reported methods for the production of m-diethylaminophenol are as follows. [0006] Method 1: Use phosphorous acid or triphenyl phosphite as a catalyst to catalyze the reaction of resorcinol and diethylamine at about 200°C, and the yield of m-diethylaminophenol can reach up to 58% (JP 09020739 and DE 4119595A1). The method has many by-products, high reaction temperature and other sho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/08C07C215/76
Inventor 彭文博葛新陈新志
Owner 上海鸿源鑫创材料科技有限公司
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