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Method for preparing diacetyl ethylenediamine

A technology of diacetylethylenediamine and ethylenediamine is applied in the field of preparation of diacetylethylenediamine, and can solve the problems of complex process, poor appearance quality of diacetylethylenediamine products and high production cost

Active Publication Date: 2009-04-01
ZHEJIANG JINKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Said method is complex in process, high in production cost, and the appearance quality of diacetylethylenediamine product is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 108g of acetic acid, 0.5g of phosphoric acid, and 100g of butyl acetate into a 500ml four-necked bottle, and mix well.

[0020] Control the temperature at 25-80°C, slowly add 45g of ethylenediamine dropwise to the above-mentioned acetic acid solution with a constant pressure funnel, then stir and raise the temperature to reflux, keep warm for 1 hour, and then dehydrate until no water occurs.

[0021] Under the condition of stirring, the dehydrated reaction material was cooled to 25°C, and after the solid was precipitated, suction filtration was performed, and the filtrate was reused as mother liquor; the obtained solid was dried to obtain 106.5 g of diacetylethylenediamine product.

[0022] After the mother liquor is reused for 10 times, the color is obviously darkened. Add zinc powder equivalent to 1.5% of the weight of the mother liquor and react at 100°C for 30 minutes. The filtered filtrate can be used as a new mother liquor for further recycling.

Embodiment 2

[0024] Add 108g of acetic acid, 0.9g of p-toluenesulfonic acid, and 100g of butyl acetate into a 500ml four-necked bottle, and mix well.

[0025] Control the temperature at 25-80°C, slowly add 45g of ethylenediamine dropwise to the above-mentioned acetic acid solution with a constant pressure funnel, then stir and raise the temperature to reflux, keep warm for 1 hour, and then dehydrate until no water occurs.

[0026] Under the condition of stirring, the dehydrated reaction material was cooled to 25°C, and after the solid was precipitated, suction filtration was performed, and the filtrate was reused as mother liquor; the obtained solid was dried to obtain 107.2 g of diacetylethylenediamine product with a purity of 99.1%.

[0027] After the mother liquor is recycled for 10 times, the color is obviously darkened, adding aluminum powder equivalent to 1% of the weight of the mother liquor, reacting at 80°C for 60 minutes, and the filtrate obtained by filtering can be used as a new...

Embodiment 3

[0029] Add 100 g of acetic acid, 0.9 g of p-toluenesulfonic acid, and 150 g of a mixed solvent (toluene:butyl acetate=50:50, wt%) into a 500 ml four-necked flask, and mix well.

[0030] Control the temperature at 25-80°C, slowly add 45g of ethylenediamine dropwise to the above-mentioned acetic acid solution with a constant pressure funnel, then stir and raise the temperature to reflux, keep warm for 1 hour, and then dehydrate until no water occurs.

[0031] Under the condition of stirring, the dehydrated reaction material was cooled to 25°C, and after the solid was precipitated, suction filtration was performed, and the filtrate was reused as mother liquor; the obtained solid was dried to obtain 105.5 g of diacetylethylenediamine product.

[0032] After the mother liquor is recycled for 10 times, the color is obviously darkened. Add zinc powder equivalent to 2.0% of the weight of the mother liquor and react at 100°C for 40 minutes. The filtered filtrate can be used as a new mot...

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PUM

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Abstract

The invention discloses a method for preparing diacetyl ethylene diamine. The method includes the following steps: a. a catalyst and a dehydrating agent are added into an acetic acid and mixed evenly with the acetic acid; b. the temperature is controlled to be between 25 and 80 DEG C and the ethylene diamine is dropped in the acetic acid solvent obtained in the step a, wherein the molar ratio between the ethylene diamine and the acetic acid is 1:2 to 2.5; c. the mixed liquid is stirred and heated for reflux and the temperature is preserved for one hour and then dehydrated; and d. a dehydratedreagent is cooled to 25 DEG C and is extracted and filtered after solids are precipitated; a filtrate is recycled; an obtained solid is dried to obtain the diacetyl ethylene diamine. The process of the method is simple; the manufacturing cost is low and the product quality is good; and the permeation rate of the mother liquid decolorized by reducing agents is enhanced dramatically, thus being capable of increasing the application times and reducing the manufacturing cost.

Description

technical field [0001] The invention belongs to the technical field of preparation of amine compounds in organic chemistry, in particular to a preparation method of diacetylethylenediamine. Background technique [0002] Tetraacetylethylenediamine (TAED) is a bleaching activator that can react sodium percarbonate and sodium perborate at room temperature, and is an activator that can adapt to low-temperature bleaching, while diacetylethylenediamine (DAED ) is an important intermediate of this activator. [0003] At present, toluene is mainly used as the dehydrating agent of diacetylethylenediamine in the production process of diacetylethylenediamine, and the dehydration time is longer (generally needs more than 10 hours). Especially as the mother liquor reuse times increase, the transmittance of the mother liquor gradually decreases, and the color of the obtained diacetylethylenediamine product also becomes darker, which affects the appearance quality of the product, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/36C07C231/02
Inventor 张招福任玉杰芦鸿武张艳阳
Owner ZHEJIANG JINKE CHEM
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