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Synthesis method of N-ethylaniline

A synthesis method and technology of ethylaniline, applied in the synthesis field of N-ethylaniline, can solve the problems of difficult separation of target product, reduced separation difficulty, high temperature and high pressure, etc., and can solve the problems of equipment corrosion, reduced separation difficulty and low cost. Effect

Active Publication Date: 2015-06-03
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is carried out at normal pressure and lower temperature, using alcohol-water mixture as the reaction solvent, its subsequent treatment is relatively simple, the difficulty of separation is greatly reduced, and the problems of acid pollution, difficult separation of target products, high temperature and high pressure are effectively solved

Method used

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  • Synthesis method of N-ethylaniline

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Effect test

Embodiment 1

[0028] A kind of synthetic method of N-ethylaniline, take aniline, acetaldehyde and hydrogen donor as basic reaction raw materials, add catalyst and alcohol in the reaction system, use alcohol-water mixed solution as solvent, carry out in ultrasonic cleaning agent reactor ;

[0029] The parameters of ultrasonic response are: working frequency: 22KHz, ultrasonic power: 200W, horn: Φ10mm.

[0030] Its concrete preparation steps are:

[0031] (1) Fix a 250mL four-neck flask in an ultrasonic reactor, add 0.08g of palladium carbon and 16.00g of methanol into the flask, stir and activate at normal temperature and pressure for 30min, wherein the stirring is magnetic stirring, and the stirring speed is 70r / min;

[0032] (2) Add 4.41g of ammonium formate and 6.51g of aniline to the above reactor, turn on the ultrasound, add dropwise a mixture of 66.00g of ethanol and 11.00g of water dissolved in 3.08g of acetaldehyde under 70r / min magnetic stirring, and the dropping time 30min, dropw...

Embodiment 2

[0035] A kind of synthetic method of N-ethylaniline, take aniline, acetaldehyde and hydrogen donor as basic reaction raw materials, add catalyst and alcohol in the reaction system, use alcohol-water mixture as solvent, and immerse the reactor in the acoustic horn in progress;

[0036] Among them, the parameters of ultrasonic response are: working frequency: 23KHz, ultrasonic power: 800W, horn: Φ10mm.

[0037] Its concrete preparation steps are:

[0038] (1) Fix a 250mL four-neck flask in an ultrasonic reactor, and add 0.216gNi-Mn / Al to the flask 2 o 3 and 21.00 g of ethanol, stirred and activated at normal temperature and pressure for 20 minutes, wherein the stirring was magnetic stirring, and the stirring speed was 100 r / min;

[0039] (2) Add 19.25g of ammonium acetate and 4.65g of aniline to the above reactor, turn on the ultrasound, add dropwise a mixture of 33.00g of methanol and 11.00g of water dissolved in 4.40g of acetaldehyde under 100r / min magnetic stirring, and th...

Embodiment 3

[0042]A kind of synthetic method of N-ethylaniline, take aniline, acetaldehyde and hydrogen donor as basic reaction raw materials, add catalyst and alcohol in the reaction system, use alcohol-water mixed liquid as solvent, carry out in cup type ultrasonic reactor ;

[0043] Among them, the parameters of ultrasonic response are: working frequency: 24KHz, ultrasonic power: 500W, horn: Φ10mm.

[0044] Its concrete preparation steps are:

[0045] (1) Fix a 250mL four-neck flask in an ultrasonic reactor, and add 0.33gNi-Co / Al to the flask 2 o 3 and 82.50 g of ethanol, stirred and activated at normal temperature and pressure for 40 minutes, wherein the stirring was magnetic stirring, and the stirring speed was 80 r / min;

[0046] (2) Introduce 0.6mol of hydrogen into the above reactor, add 9.30g of aniline, turn on the ultrasound, add dropwise a mixture of 22.00g of isopropanol and 11.00g of water dissolved in 6.60g of acetaldehyde under 80r / min magnetic stirring, drop Adding tim...

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Abstract

The invention discloses a synthesis method of an N-ethylaniline, which is characterized in that aniline, acetaldehyde and a hydrogen donor are used as basic reaction raw materials, catalyst and alcohol are added in the reaction system, alcohol-water mixed liquid is adopted as a solvent, and the reaction is carried out in an ultrasonic reactor. According to the synthesis method, aniline, acetaldehyde and the hydrogen donor are used as raw materials and the alcohol-water mixed liquid is used as the solvent, so that the problem of the acid pollution and equipment corrosion can be effectively solved; and moreover, the environmental pollution is hardly caused, the cost is low, the subsequent processing is relatively simple, the separation difficulty is greatly lowered, and the yield of the product is high. N-ethylaniline is synthesized by adopting the ultrasonic reactor, so that the synthesis of N-ethylaniline can be carried out under the normal pressure and a low temperature, the production cost can be effectively reduced, and the requirement on the equipment can be lowered.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis method of N-ethylaniline. Background technique [0002] N-Ethylaniline, also known as ethylaniline, English name N-Ethylanlllne, yellow-brown transparent oily liquid with aniline smell, boiling point 204°C, insoluble in water, soluble in alcohol and most organic solvents. N-Ethylaniline is a very important chemical intermediate, which can be used as an intermediate of various dyes, and can also be used as a raw material for products such as pesticides, medicines, rubber additives, and photosensitive materials. At the same time, in recent years, many companies have used it as an antiknock agent and antioxidant for the gasoline industry. [0003] At present, the production methods of N-ethylaniline are mainly liquid phase method and gas phase method. The liquid phase method has disadvantages such as severe equipment corrosion, high equipment cost, high operating press...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/48C07C209/28C07C209/26
Inventor 马韵升栾波汪正安吴文雷姚刚樊其艳
Owner CHAMBROAD CHEM IND RES INST CO LTD