Preparation method of 3-chloro-2,6-diethyl aniline

A technology of diethylaniline and chloroaniline, applied in chemical recovery, organic chemistry, etc., can solve problems such as pollution, low product yield, poor quality performance, etc., and achieve the effect of simple process, high product quality and stable reaction

Inactive Publication Date: 2007-01-31
黄秋耉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method overcomes the toxicity and corrosivity brought by the use of chlorine in the prior art, the instability of the raw material 2,6-die

Method used

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  • Preparation method of 3-chloro-2,6-diethyl aniline
  • Preparation method of 3-chloro-2,6-diethyl aniline
  • Preparation method of 3-chloro-2,6-diethyl aniline

Examples

Experimental program
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Effect test

Embodiment 1

[0033] In a 2000ml pressure vessel with electric heating and coil cooling, add 500 grams of aniline and 20 grams of metal aluminum powder, and feed nitrogen to replace the air in the vessel. After the container is sealed, heat it up to 260°C. When the temperature is high, turn on the cooling oil to cool down. Stir at a constant temperature of 260°C for 2 hours, and then cool to room temperature. Open the container and vent to remove the hydrogen gas formed. Add 500 grams of m-chloroaniline from the feeding port, heat up the container to 300 ° C after sealing, open the ethylene valve, press ethylene into the container, keep the pressure at 15 MPa, control the ethylene addition rate at 2 to 4 g / min, and wait until the pressure of the reaction container When rising to 16MPa, slow down the feeding speed of ethylene, and the speed is controlled at 1-2 g / min. When the pressure of the reaction vessel rises to 18MPa, stop adding ethylene, and the reaction ends. The ethylation / displac...

Embodiment 2

[0037] In a 2000ml pressure vessel with electric heating and coil cooling, add 500 grams of o-toluidine and 20 grams of metal aluminum, and feed nitrogen to replace the air in the vessel. After the container is sealed, heat it up to 300°C. When the temperature is high, turn on the cooling oil to cool it. Stir at a constant temperature of 300°C for 2 hours, and then cool to room temperature. Open the container and vent to remove the hydrogen gas formed. Add 500 grams of m-chloroaniline from the feeding port, heat up the container to 300 ° C after sealing, open the ethylene valve, press ethylene into the container, keep the pressure at 15 MPa, control the ethylene addition rate at 2 to 4 g / min, and wait until the pressure of the reaction container When rising to 16MPa, slow down the feeding speed of ethylene, and the speed is controlled at 1-2 g / min. When the pressure of the reaction vessel rises to 18MPa, stop adding ethylene, and the reaction ends. The reaction temperature is...

Embodiment 3

[0041] In a 2000ml pressure vessel with electric heating and coil cooling, add 450 grams of o-toluidine, add 25 grams of zinc, and add nitrogen to replace the air in the vessel. After sealing the container, heat up to 250°C, stir at constant temperature for 2 hours, and then cool to normal temperature. Open the container and vent to remove the hydrogen gas formed. Add 495 grams of m-chloroaniline from the feeding port, raise the temperature to 310°C, open the ethylene valve, press ethylene into the container, keep the pressure at 14MPa, control the ethylene addition rate at 2-4 g / min, and wait until the pressure of the reaction container rises to 15MPa Slow down the feeding speed of ethylene, and the speed is controlled at 1 to 2 g / min. When the pressure of the reaction vessel rises to 18MPa, the feeding of ethylene is stopped, and the reaction ends. The reaction temperature is controlled at 310°C±10°C.

[0042] After the reaction, cool down to 95°C, open the feeding and ven...

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Abstract

The present invention discloses a preparation method of 3-chloro-2,6-diethylaniline. Said method includes the following steps: heating metal or its salt in aniline or alkylaniline and making them produce reaction to obtain aniline or alkylaniline metal complex catalyst, adding m-chloroaniline into the obtained complex catalyst, under the condition of 150deg.C-400deg.C and 10MPa-25MPa introducing ethylene, under the action of aniline or alkylaniline metal complex catalyst producing ethylated complex, then making m-chloroailine and ehylated complex produce metathetical reaction so as to obtain 3-chloro-2,6-diethylaniline, and make the complex catalyst obtain regeneration.

Description

technical field [0001] The invention relates to a preparation method of 3-chloro-2,6-diethylaniline. Background technique [0002] The research and development of polyurethane (referred to as PU) materials has a history of more than 60 years. In recent years, with the continuous expansion of the application of PU materials, the number of its products has leapt to the top of the world's six major synthetic materials, and the global output is more than 1,000 About ten thousand tons. [0003] Due to its excellent performance, PU materials are widely used in various fields of the national economy and in all aspects of people's basic necessities of life. PU materials are generally formed by polycondensation of polyether or polyester polyols and polyisocyanates. In order to expand the application range of PU materials and improve their various physical properties, small molecules called "chain extenders" are added to the PU synthesis process. Materials, such as polyols, fatty al...

Claims

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Application Information

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IPC IPC(8): C07C211/52
CPCY02P20/584
Inventor 黄秋耉黄斌
Owner 黄秋耉
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