Preparation method of N1-(2-aminoethyl)-1, 2-ethylenediamine

An ethylenediamine and aminoethyl technology, which is applied in the field of preparation of N1--1,2-ethylenediamine (DETA), can solve the problems of process corrosion, deactivation, and high equipment investment, and save equipment investment and energy. The effect of reducing energy consumption, reducing pressure, reducing energy consumption and equipment investment

Active Publication Date: 2014-02-26
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The dichloroethane method adopts a liquid phase environment, the process is severely corroded, the product is difficult to separate, and a large amount of amine-containing wastewater will be generated, which is difficult to treat, high in energy consumption, and seriously pollutes the environment.
Because aminoacetonitrile is easy to polymerize and decompose at room temperature, unnecessary impurities are introduced to cause complex and changeable components in the product, and the unstable composition of the reaction solution is not conducive to the subsequent separation of various vinylamines. In addition, the HCN decomposed by aminoacetonitrile is also It will lead to the reduction or even deactivation of the catalyst activity
[0007] The prior art has disadvantages such as low yield of DETA, difficult separation of products, easy deactivation of catalyst, high energy consumption and high equipment investment.

Method used

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  • Preparation method of N1-(2-aminoethyl)-1, 2-ethylenediamine
  • Preparation method of N1-(2-aminoethyl)-1, 2-ethylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0035] use as figure 1 The reaction setup shown was used for this example. Both the first hydrogenation reactor and the second hydrogenation reactor are stainless steel tubular reactors of φ10mm×400mm. The first hydrogenation reactor was filled with 50 g of ETH-2000 from Datong Universal Chemical Co., Ltd. with a particle size of 2 mm. Fill the second hydrogenation reactor with 50 g of Raney 5886 from Grace Company with a particle size of 1-3 mm. Reaction system reaction pressure is controlled at 8Mpa, and the IDAN dioxane solution of 15wt% is with the rate of 100g / h, and the rate of 0.1wt% dioxane hydrochloride solution is with 6g / h, and hydrogen is with the rate of 450 standard liters / h Continuously enter the first hydrogenation reactor. The temperature of the first hydrogenation reaction is controlled at 100°C to obtain the first hydrogenation reaction liquid, the first hydrogenation reaction liquid and 0.15wt% sodium hydroxide dioxane solution continuously enter the sec...

Embodiment 2

[0037] use as figure 1 The reaction setup shown was used for this example. Both the first hydrogenation reactor and the second hydrogenation reactor are stainless steel tubular reactors of φ10mm×400mm. The two-stage hydrogenation reactors were filled with 50 g of Raney 2786 from Grace Company with a particle size of 0.6-3 mm. The reaction system reaction pressure is controlled at 6Mpa, and the IDAN dioxane solution of 5wt% is with the rate of 450g / h, and the dioxane hydrochloride solution of 1wt% is with the rate of 6g / h, and hydrogen is continuous with the rate of 500 standard liters / h into the first hydrogenation reactor. The first reaction temperature is controlled at 120°C to obtain the first hydrogenation reaction liquid, the first hydrogenation reaction liquid and 1wt% sodium hydroxide dioxane solution enter the second hydrogenation reactor from the top of the second hydrogenation reactor , the flow rate of the sodium hydroxide dioxane solution was 9 g / h, and the seco...

Embodiment 3

[0039] use as figure 1 The reaction setup shown was used for this example. Both the first hydrogenation reactor and the second hydrogenation reactor are stainless steel tubular reactors of φ10mm×400mm. The first hydrogenation reactor was filled with 50 g of Raney 5831 from Grace Company with a particle size of 2 mm. The ACTICAT of CatAlloy Company with a particle size of 1-4mm is filled in the second hydrogenation reactor TM 3400. Reaction system reaction pressure is controlled at 10Mpa, and the IDAN dioxane solution of 15wt% is with the speed of 140g / h, and the speed of 0.5wt% dioxane hydrochloride solution is with 7g / h, and hydrogen is with the speed of 450 standard liters / h Continuously enter the first hydrogenation reactor. The temperature of the first hydrogenation reaction is controlled at 90°C to obtain the first hydrogenation reaction liquid, and the first hydrogenation reaction liquid and 0.5wt% sodium hydroxide dioxane solution enter the second hydrogenation reac...

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Abstract

The invention provides a preparation method of N1-(2-aminoethyl)-1, 2-ethylenediamine (DETA). The method comprises the steps: (1) carrying out a first hydrogenation reaction on an iminodiacetonitrile (IDAN) solution, an acid additive and hydrogen under the catalysis of a first hydrogenation catalyst to obtain a first hydrogenation reaction liquid; and (2) carrying out second hydrogenation reaction on the first hydrogenation reaction liquid, an alkaline additive and the hydrogen under the catalysis of a second hydrogenation catalyst to obtain a DETA reaction liquid. Compared with the prior art, the method provided by the invention has the advantages that the conversion ratio of the IDAN can be greatly increased; the yield of the target product is greatly increased; the stability of the catalyst is increased.

Description

technical field [0001] The present invention relates to a kind of N 1 -(2-aminoethyl)-1,2-ethylenediamine (DETA) preparation method, more specifically relates to a two-step hydrogenation preparation method for DETA. Background technique [0002] N 1 -(2-aminoethyl)-1,2-ethylenediamine, molecular formula C 4 h 13 N 3 , referred to as DETA, commonly known as diethylenetriamine, diethylenetriamine, diethylenetriamine, diethylenetriamine, etc., English name: Diethylenetriamine, is a saturated fatty amine, yellow hygroscopic transparent viscous liquid , has a pungent ammonia odor, and easily absorbs moisture and carbon dioxide in the air. It is mainly used as a solvent and organic synthesis intermediate, and can be used to prepare carbon dioxide absorbers, lubricating oil additives, emulsifiers, photographic chemicals, surfactants, fabric finishing agents, paper strengthening agents, ammonia carboxy complexing agents, ashless additives , metal chelating agent, heavy metal h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/14C07C209/48
Inventor 丁可陈长生李付国李昂崔兵黎源
Owner WANHUA CHEM GRP CO LTD
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