Method for synthesizing diethyltoluenediamine

A technology of diethyltoluenediamine and diaminotoluene, which is applied in the field of synthesizing diethyltoluenediamine, can solve the problems of catalysts not being reused, increasing the pressure of environmental protection, reaction temperature, high pressure, etc., and achieve the realization of recycling The effect of streamlining production, saving energy and improving production efficiency

Active Publication Date: 2016-11-09
山东崇舜新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing diethyltoluenediamine synthesis method has high reaction temperature and pressure; no catalyst is used or the catalytic system is poisonous and flammable; some processes use organic solvents, and some have alkali washing and water washing links, adding lye to destroy the catalytic system
At the same time, the catalyst has not been reused, which not only increases the cost but also increases the pressure of environmental protection

Method used

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  • Method for synthesizing diethyltoluenediamine
  • Method for synthesizing diethyltoluenediamine

Examples

Experimental program
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Effect test

example 1

[0023] ①Add 1500g of diaminotoluene and catalyst (30g of aluminum powder, 14g of zinc powder, 45g of anhydrous aluminum trichloride, 0.5g of diethylaluminum chloride) into a 5L reactor, protect it with dry nitrogen, and slowly raise the temperature to 180°C And maintain the reaction at 180-200°C for 1.5 hours.

[0024] ② Use ethylene to drive out the hydrogen and nitrogen in the kettle and pressurize to 1.0MPa. When the temperature rises to 267°C, the pressure begins to drop and the alkylation reaction begins. Control the ethylene pressure at 4.0MPa through a pressure reducing valve and a flow meter. The temperature is controlled between 270-290°C. After 4.6 hours of reaction, the temperature stabilizes and drops slightly, and the ethylene pressure no longer drops, and the reaction is considered to be over.

[0025] ③After the pressure is released, put it into a retort for distillation. After cutting off about 10% of the front fraction, distill 1200g of the main fraction with ...

example 2

[0030] ①Put 250KG of raw material diaminotoluene (TDA) into a 500L kettle, add 5.0KG of aluminum powder, 1.50KG of zinc powder, and 7.5KG of anhydrous aluminum trichloride, and react at 114-200°C for 2.5 hours.

[0031] ②Press dry nitrogen into a 500L high-pressure reactor, replace it with ethylene three times, pressurize to 1.0MPa, start to heat up, and the pressure in the autoclave starts to drop at 261°C, and the alkylation reaction starts, adjust the ethylene flow rate to control the inside of the reactor The pressure was 4.0 MPa, the reaction temperature was 265-275°C, after 3.5 hours of reaction, the pressure stopped dropping and remained for 0.5 hours, the temperature stabilized and dropped slightly, and the alkylation reaction ended.

[0032] ③Unload and recover ethylene, until the pressure in the kettle drops to 0.4MPa, the material enters the still still for distillation, and the main fraction of 202KG is distilled, with a diamine content of 99.7%, and the fraction be...

Embodiment 3

[0037] The catalytic system residue generated by the final application of Example 1 and Example 2 is washed with a polar solvent and separated. The organic phase is polyamine, which is used as a curing agent in the bottom material of the PU track.

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Abstract

The invention discloses a method for synthesizing diethyltoluenediamine. An arylamine-aluminum catalyst system is formed with diaminotoluene under certain conditions, then, an alkylation reaction with ethylene is carried out in an autoclave, a reaction product directly enters a distillation still for distillation after the reaction ends, a front cut fraction and a remaining catalyst system directly return to the autoclave, then, the raw material diaminotoluene is put into the autoclave and is subjected to an alkylation reaction with ethylene directly, and the arylamine-aluminum catalyst system can be reused through one-time preparation. Meanwhile, a straight distillation technology is adopted, so that the consumption of organic solvents is avoided, the purity of the product can be higher, and the production process is more environmentally friendly. According to the synthesis method, the catalyst system is reused repeatedly, and the process is free of solvents and neutralizing and washing processes, so that the production cost is reduced, the production efficiency is increased, and process flows are simpler, safer and more environmentally friendly.

Description

technical field [0001] The invention relates to the field of alkylation reactions of aromatic amines, in particular to a method for synthesizing diethyltoluenediamine. Background technique [0002] Diethyltoluenediamine, abbreviated as DETDA, the product name is Ethacure○R100, referred to as E100, is a fast amine chain extender, mainly used in polyurethane and epoxy resin curing agent, and can also be used as an oil chemical intermediate In recent years, with the promotion and use of high-speed rail technology, reaction injection molding and spray polyurea in polyurethane have developed rapidly, and diethyltoluenediamine has been widely used as an ideal raw material for spray polyurea. [0003] The existing diethyltoluenediamine synthesis method has high reaction temperature and pressure; no catalyst is used or the catalytic system is poisonous and flammable; some processes use organic solvents, and some processes have alkali washing and water washing steps, adding alkali to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C211/51
CPCC07C209/68C07C211/51
Inventor 杨申钟文清陈南超李金木
Owner 山东崇舜新材料科技有限公司
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