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Tris(2-aminoethyl)amine synthesis process

A technology of aminoethyl and synthesis process, which is applied in the field of triamine synthesis process, can solve the problems of harm to human body and environment, cumbersome operation, low yield, etc., and achieve low harm to human body and environment, short process flow and low production cost Effect

Active Publication Date: 2019-03-08
安徽工业大学科技园有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current traditional synthesis process not only has the disadvantages of many raw materials, cumbersome operation, and low yield, but also produces toxic by-products that are harmful to the human body and the environment.

Method used

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  • Tris(2-aminoethyl)amine synthesis process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 14.9g of triethanolamine solution and 29.8g of DMF into a 500ml three-necked flask, stir, take 50g of thionyl chloride solution, and slowly add it dropwise to the above reagents, and the dropping speed is controlled at 1 second per drop. At first there was a white solid accompanied by gas generation, but after the dropwise addition, the white solid disappeared and the solution was clear. Stirring was continued for 7 hours. Reflux reaction at 70°C for 6-8 hours to obtain the first intermediate tris(2-chloroethyl)amine hydrochloride. After the reaction, tris(2-chloroethyl)amine hydrochloride produced by rotary evaporation under reduced pressure salt, remove the remaining thionyl chloride solution to obtain tris(2-chloroethyl)amine hydrochloride concentrate.

[0026] Add tris(2-chloroethyl)amine hydrochloride concentrate and 35g ammonia water into a 1000ml three-neck flask, add 100g ethanol to dissolve it, stir, and heat in an oil bath to 70°C, keep the solution refl...

Embodiment 2

[0028] Take 14.9g of triethanolamine solution and 14.9g of DMF into a 1000ml three-necked flask, stir, take 50g of thionyl chloride solution, and slowly add it dropwise to the above reagents, and the dropping speed is controlled at 1 second per drop. At first there was a white solid accompanied by gas generation, but after the dropwise addition, the white solid disappeared and the solution was clear. Stirring was continued for 7 hours. After the reaction was completed, the generated tris(2-chloroethyl)amine hydrochloride was rotary evaporated under reduced pressure, and the remaining thionyl chloride solution was removed to obtain a concentrated solution of tris(2-chloroethyl)amine hydrochloride.

[0029] Add the above concentrate and 70g of ammonia water into a 1000ml three-neck flask, add 100g of ethanol to dissolve it, stir, and heat in an oil bath to 70°C, keep the solution at reflux, and react at reflux for 7 hours. The color of the reaction solution gradually changed fr...

Embodiment 3

[0031] Take 14.9g of triethanolamine solution and 21g of DMF into a 1000ml three-necked flask, stir, take 50g of thionyl chloride solution, and slowly add it dropwise to the above reagent, and the dropping speed is controlled at 1 second per drop. At first there was a white solid accompanied by gas generation, but after the dropwise addition, the white solid disappeared and the solution was clear. Stirring was continued for 7 hours. After the reaction was completed, the generated tris(2-chloroethyl)amine hydrochloride was rotary evaporated under reduced pressure, and the remaining thionyl chloride solution was removed to obtain a concentrated solution of tris(2-chloroethyl)amine hydrochloride.

[0032] Add the above concentrated solution and 140g ammonia water into a 1000ml three-necked flask, add 100g ethanol to dissolve it, stir, and heat in an oil bath to 70°C, keep the solution under reflux, and react under reflux for 7 hours. The color of the reaction solution gradually ...

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Abstract

The invention discloses a tris(2-aminoethyl)amine synthesis process, and belongs to the technical field of compound preparation. The tris(2-aminoethyl)amine synthesis process includes the steps of taking triethanolamine as a starting material, putting the triethanolamine, thionyl chloride and a catalyst DMF in a reactor, heating the three to generate tris(2-chloroethyl)amine hydrochloride, dissolving separated tris(2-chloroethyl)amine hydrochloride concentrate and ammonia water in an organic solvent in a reactor, putting the solution in the reactor, carrying out a reaction while heating to obtain tris(2-aminoethyl)amine hydrochloride, and reacting the tris(2-aminoethyl)amine hydrochloride with sodium hydroxide to obtain the tris(2-aminoethyl)amine. The tris(2-aminoethyl)amine synthesis process has the advantages of short reaction route and high controllability.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to the technical field of synthesis of aliphatic nitrogen-tritium tetramine, in particular to a synthesis process of tris(2-aminoethyl)amine. Background technique [0002] Tris(2-aminoethyl)amine, the structural formula is as follows: [0003] [0004] Aliphatic nitrogen-tritium tetramine can be used in research and industrial fields such as chelating agent, corrosion inhibitor, resin curing agent, catalyst, organic intermediate, etc. Tris (2-aminoethyl) amine is one of the aliphatic nitrogen-tritium tetramine compounds An important organic polyamine compound. Its outstanding structural feature is that there are four nitrogen atoms with strong coordination ability in the molecule, which can be combined with most transition metal atoms (such as Cd 2+ , Zn 2+ , Mn 2+ etc.) to form a stable chelate with a bicyclic structure. [0005] In addition, aliphatic nitrogen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/16C07C211/15C07C209/00C07C211/14
CPCC07C209/00C07C209/16C07C211/15C07C211/14
Inventor 叶明富夏国威许立信宋丰发万超
Owner 安徽工业大学科技园有限公司
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